Share a compound : Application of 10320-42-0

At the same time, in my other blogs, there are other synthetic methods of this type of compound,10320-42-0, 2-Chloro-5-nitropyrimidine, and friends who are interested can also refer to it.

Application of 10320-42-0, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 10320-42-0, name is 2-Chloro-5-nitropyrimidine. A new synthetic method of this compound is introduced below.

(3S)-1o-(3-aminopyrrolidin- 1-yl)-9-fluoro-3-methyl-7-oxo-2,3-dihydro-7H- [1,4]oxazino[2,3,4-ij]quinoline-6-carboxylic acid (40 mg, 0.115 mmol, 1 eq) was dissolved in dimethyl sulfoxide (2 mL) with 2-Chloro-5-nitropyflmidine (36.74 mg, 0.230 mmol, 2 eq) in a s mL capacity microwave vessel fitted with a magnetic stirrerbar and microwaved at 160¡ãC for 1.5 hours. The DMSO was evaporated the compound was crystalized using hot ethanol to afford compound A1.27. 1H NMR (400 MHz, DMSO-d6) 6 15.38 (br. s., 1H), 9.15 (d, J = 3.30 Hz, 1H), 9.08 (d, J= 3.30 Hz, 1H), 8.90 (s, 1H), 7.56 (d, J = 14.12 Hz, 1H), 4.90-4.85 (m, 1H), 4.60 – 4.56 (m, 1H), 4.53 (d, J = 11.74 Hz, 1H), 4.28 (d, J = 11.19 Hz, 1H), 4.05 ? 3.90 (m, 2H), 3.75 – 3.83-3.68 (m, 2H), 2.22 (tcl, J = 6.53, 12.79 Hz, 1H), 2.05 (dcl, J = 6.51, 12.56 Hz, 1H),1.45 (ci, J = 6.79 Hz, 3H); Formula C21H19FN606 LC-MC Retention time 3.362 mm,Found 471.1 [M+H]

At the same time, in my other blogs, there are other synthetic methods of this type of compound,10320-42-0, 2-Chloro-5-nitropyrimidine, and friends who are interested can also refer to it.

Reference:
Patent; KING’S COLLEGE LONDON; THE SECRETARY OF STATE FOR HEALTH; RAHMAN, Khondaker Mirazur; JAMSHIDI, Shirin; LAWS, Mark Benjamin; NAHAR, Kazi; SUTTON, John Mark; HIND, Charlotte; (265 pag.)WO2018/220365; (2018); A1;,
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Simple exploration of Safety of 2,5-Dichloro-N-(2-(isopropylsulfonyl)phenyl)pyrimidin-4-amine

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 761440-16-8, 2,5-Dichloro-N-(2-(isopropylsulfonyl)phenyl)pyrimidin-4-amine.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 761440-16-8, name is 2,5-Dichloro-N-(2-(isopropylsulfonyl)phenyl)pyrimidin-4-amine. A new synthetic method of this compound is introduced below., Safety of 2,5-Dichloro-N-(2-(isopropylsulfonyl)phenyl)pyrimidin-4-amine

Isopropanol (445 kg) was added to 2,5-dichloro-N-(2-(isopropylsulfonyl)phenyl)pyrimidin-4-amine (70.2 kg, 203 mol, 1.15 eq.) and 2-Isopropoxy-5-methyl-4-(piperidin-4-yl)aniline dihydrochloride (56.7 kg, 176 mol). The mixture was heated for approx. 16 hours at reflux. Water (47 kg) was added and the mixture cooled to 0 C. The solid was filtered and washed with isopropanol/water. To the wet product, isopropanol (680 kg) and water (55 kg) was added and the slurry heated to reflux. The obtained clear solution was cooled to 0 C., filtered and dried under vacuum to yield 5-chloro-N2-(2-isopropoxy-5-methyl-4-(piperidin-4-yl)phenyl)-N4-(2-(isopropylsulfonyl)phenyl)pyrimidine-2,4-diamine dihydrochloride (=ceritinib dihydrochloride; 84.5 kg [t.q., contains 10% w/w isopropanol], 76.0 kg [100%], 68% yield). Ethanol (155 kg) and water (113 kg) were added to 5-chloro-N2-(2-isopropoxy-5-methyl-4-(piperidin-4-yl)phenyl)-N4-(2-(isopropylsulfonyl)phenyl)pyrimidine-2,4-dihydrochloride; 45.0 kg [t.q., contains 10% w/w isopropanol], 40.5 kg [100%], 64.2 mol) and the mixture heated to 55 C. Aqueous NaOH (147 L of a 1 M solution, 2.3 eq.) was added slowly and then cooled to 20 C. After filtration, the product was recrystallized from ethanol and dried under vacuum to yield ceritinib (33.2 kg, 93% yield based on ceritinib dihydrochloride) as an almost white powder. 1H-NMR (400 MHz, CDCl3): delta=1.33 (d, J=6.8 Hz, 6H), 1.38 (d, J=6.1 Hz, 6H), 1.59-1-78 (m, 5H), 2.18 (s, 3H), 2.75-2.83 (m, 3H), 3.20-3.24 (m, 2H), overlaps 3.28 (sept, J=6.8 Hz, 1H), 4.56 (sept, J=6.1 Hz, 1H), 6.82 (s, 1H), 7.25-7.29 (m, 1H), 7.56 (br. s, 1H), 7.64 (m, 1H), 7.94 (m, 1H), 8.01 (br. s, 1H), 8.16 (br. s, 1H), 8.60 (m, 1H), 9.51 (br. s, 1H) ppm. 13C-NMR (100 MHz, CDCl3): delta=15.4, 18.9, 22.3, 33.9, 38.6, 47.5, 55.4, 71.4, 105.7, 111.0, 120.6, 123.1, 123.7, 124.9, 126.7, 127.3, 131.2, 134.7, 138.3, 138.5, 144.7, 155.3, 155.4, 157.5 ppm, Elemental analysis: calculated (%) for C28H36ClN5O3S: C 60.26, H 6.50, N 12.55, O 8.60 Cl 6.35, S 5.74, found: C 60.15, H 6.45, N 12.72, O 8.58, Cl 6.43, S 5.67.)

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 761440-16-8, 2,5-Dichloro-N-(2-(isopropylsulfonyl)phenyl)pyrimidin-4-amine.

Reference:
Patent; Novartis AG; Davis, Mark Clinton; Gong, Baoqing; Har, Denis; Kapferer, Tobias; Zheng, Xuchun; (25 pag.)US2020/39935; (2020); A1;,
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Brief introduction of Related Products of 16357-69-0

The chemical industry reduces the impact on the environment during synthesis 16357-69-0, I believe this compound will play a more active role in future production and life.

Related Products of 16357-69-0, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.16357-69-0, name is 4-Aminopyrimidine-5-carbonitrile, molecular formula is C5H4N4, molecular weight is 120.11, as common compound, the synthetic route is as follows.

General procedure: Substrate (1.0 mmol), [HDBN+][TFE-] (6.0 mmol) were loaded in a 10 mL glass reaction tube equipped with a magnetic stirrer. The air in the reactor was replaced by CO2. Then, the reactor was stirred at the desired temperature for 3-96 h under CO2 using a balloon. After the reaction, the reaction liquid was cooled to room temperature and quenched by saturated ammonium chloride solution. Then the mixture was filtered to afford the crude product, which was purified by chromatography (silica gel, methanol/dichloromethane=1/20) to give the desired compound. The purified product was characterized by NMR and HR-MS. 1H NMR and 13C NMR studies were carried out with a JEOL NMR 400 (400 MHz, 100 MHz) spectrometer with DMSO-d6 as the solvent. Mass spectra were recorded with an AMD40223(Interambulacra) spectrometer.

The chemical industry reduces the impact on the environment during synthesis 16357-69-0, I believe this compound will play a more active role in future production and life.

Reference:
Article; Li, Chun; Lu, Xunhua; Yang, Yuanyong; Yang, Shenggang; Zhang, Lin; Tetrahedron Letters; vol. 59; 25; (2018); p. 2463 – 2466;,
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Some tips on Related Products of 7461-50-9

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 7461-50-9, 2-Chloropyrimidin-4-amine.

Related Products of 7461-50-9, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 7461-50-9, name is 2-Chloropyrimidin-4-amine. This compound has unique chemical properties. The synthetic route is as follows.

A mixture of 3-(5-aminopyrazin-2-yl)-6-cyclobutyl-2-fluorophenol (17.0 g, 65.6 mmol), K2CO3 (13.6 g, 98.4 mmol), 2-chloropyrimidin-4-amine (8.9 g, 69 mmol), 18-crown-6 (0.87 g, 3.3 mmol), and DMA (131 mL) was stirred at 120 Celsius for 15 hours. Water (306 mL) was added, and the reaction mixture cooled to room temperature. Solid precipitate was collected by vacuum filtration and dried in a vacuum oven at 70 Celsius to give the crude product (23.1 g, 100%). The solid was recrystallized from EtOH and treated successively with activated charcoal and silica-supported thiol to remove residual Pd and afford the title compound (13.0 g, 56%). MS (ESI): mass calcd. for C18H17FN6O, 352.14; m/z found, 353.2 [M+H]+. 1H NMR (500 MHz, DMSO-d6) delta 8.25 (s, 1H), 8.01 (d, J=1.5, 1H), 7.83 (d, J=5.8, 1H), 7.66 (m 1H), 7.23 (d, J=8.3, 1H), 7.06 (s, 2H), 6.67 (s, 2H), 6.17 (d, J=5.8, 1H), 3.60-3.47 (m, 1H), 2.19-2.01 (m, 4H), 1.98-1.85 (m, 1H), 1.80-1.68 (m, 1H).

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 7461-50-9, 2-Chloropyrimidin-4-amine.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; Eccles, Wendy; Fitzgerald, Anne E.; Hack, Michael D.; Hawryluk, Natalie A.; Jones, William M.; Keith, John M.; Krawczuk, Paul; Lebsack, Alec D.; Liu, Jing; Mani, Neelakandha S.; McClure, Kelly J.; Meduna, Steven P.; Rosen, Mark D.; US2015/252008; (2015); A1;,
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Some scientific research about Synthetic Route of 51940-64-8

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 51940-64-8, Ethyl 2,4-Dichloro-5-pyrimidinecarboxylate.

Synthetic Route of 51940-64-8, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 51940-64-8, name is Ethyl 2,4-Dichloro-5-pyrimidinecarboxylate, molecular formula is C7H6Cl2N2O2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

DIPEA (4.28 mL, 24.5 mmol) was added dropwise to ethyl 2,4-dichloropyrimidine-5- carboxylate (2.46 g, 11.1 mmol) and 4-amino-4-methyl-cyclohexanol hydrochloride (2.00 g, 11.1 mmol) in acetonitrile (40 mL) at 0C over 5 min. The reaction mixture was allowed to warm to rt, then was stirred at rt for 6 h and concentrated in vacuo, diluted with EtOAc (300 mL) and washed with sat. brine (100 mL x 2). The organic layer was isolated and dried over MgSC and concentrated in vacuo. The resulting crude product was purified by fee, elution gradient 0 to 20% EtOAc in n-heptane, to afford the title compound (2.82 g, 81%) as a pale yellow gum;lH NMR (400 MHz, DMSO) 1.36 – 1.44 (3H, m), 1.44 – 1.58 (6H, m), 1.57 – 1.71 (1H, m), 1.72 – 2.13 (3H, m), 2.41 – 2.54 (2H, m), 3.63 – 3.75 (1H, m), 4.36 (2H, q), 8.52 – 8.59 (1H, m), 8.67 (1H, d); mJz MH+314.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 51940-64-8, Ethyl 2,4-Dichloro-5-pyrimidinecarboxylate.

Reference:
Patent; ASTRAZENECA AB; CANCER RESEARCH TECHNOLOGY LIMITED; FINLAY, Maurice, Raymond, Verschoyle; GOLDBERG, Frederick, Woolf; TING, Attilla, Kuan, Tsuei; (103 pag.)WO2018/114999; (2018); A1;,
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Analyzing the synthesis route of Related Products of 153435-63-3

According to the analysis of related databases, 153435-63-3, the application of this compound in the production field has become more and more popular.

Related Products of 153435-63-3, Adding some certain compound to certain chemical reactions, such as: 153435-63-3, name is 2-(Tributylstannyl)pyrimidine,molecular formula is C16H30N2Sn, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 153435-63-3.

A solution of 2-tributylstannanyl pyrimidine (390 mg, 1.05 mmol) , 2-pyrimidin triflate intermediate (13) (510 mg, 0.81 mmol), and Pd(PPh3)4 (95 mg, 0.081 mmol) in dry dimethylacetamide (7.5 mL) was heated at 130C for 6 h. After being cooled to room temperature, the reaction was filtered through a plug of Celite, the filtrate was diluted with water and extracted twice with ethyl acetate. The combined organic layers were washed with brine, solvent was removed and the residue was purified by silica gel chromatography furnishing the desired compound as a pale yellow solid (357 mg, 79 %) . The crude bosentan was further purified by recrystallization in hot ?0 / EtOH affording pure bosentan monohydrate (1) as a white solid (327 mg, 70 %) .^-RMN (200 MHz, d6-DMSO) : 1.29 (s, 9H) ; 3.85 (m, 2H) ; 3.93 (s, 3H) ; 4.59 (m, 2H) ; 6.81-7.18 (m, 4H) , 7.43 (d, J = 8.0 Hz, 3H) ; 8.45 (d, J = 8.0 Hz, 2H) ; 9.01 (s, 2H) ppm.DSC-TG: endothermic peak at 116.53 C, with a loss of weight of 3.1 % (monohydrate) . Dio : 1.36 um, D50 : 20.32 muiotaeta, D90 : 56.64 muiotaeta

According to the analysis of related databases, 153435-63-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; LABORATORIOS LESVI, S.L.; RODRIGUEZ ROPERO, Sergio; HUGUET CLOTET, Juan; WO2011/117143; (2011); A1;,
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New learning discoveries about Quality Control of 6-Chloro-5-iodopyrimidin-4-amine

At the same time, in my other blogs, there are other synthetic methods of this type of compound,353272-15-8, 6-Chloro-5-iodopyrimidin-4-amine, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 353272-15-8, 6-Chloro-5-iodopyrimidin-4-amine, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, Quality Control of 6-Chloro-5-iodopyrimidin-4-amine, blongs to pyrimidines compound. Quality Control of 6-Chloro-5-iodopyrimidin-4-amine

Compound (S)-3-(1-Aminoethyl)-2-cyclopropyl-8-fluoroisoquinolin-1(2H)-one (425 mg, 1.726 mmol),6-chloro-5-iodopyrimidine-4-amine (463.8 mg, 1.816 mmol) andA mixture of DIPEA (445.5 mg, 3.447 mmol) in n-butanol (2.5 mL) was heated to 130 C and stirring was continued for 30 hours.After cooling to room temperature and concentrating under reduced pressure, EtOAc m.The crude product was purified by silica gel column chromatography (EtOAc/EtOAc)The title compound was obtained as a pale yellow solid (250 mg, 31%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,353272-15-8, 6-Chloro-5-iodopyrimidin-4-amine, and friends who are interested can also refer to it.

Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Jiatuo Sciences Corporation; Xi Ning; Wang Liang; Wang Tingjin; Wu Weibin; (84 pag.)CN105130966; (2019); B;,
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The origin of a common compound about Reference of 18592-13-7

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 18592-13-7, 6-(Chloromethyl)pyrimidine-2,4(1H,3H)-dione.

Reference of 18592-13-7, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 18592-13-7, name is 6-(Chloromethyl)pyrimidine-2,4(1H,3H)-dione. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: The respective halomethyl derivatives {6-(chloromethyl)uracil (0.1150g, 0.716mmol) or 4-bromomethyl-7-methoxycoumarin (0.1928g, 0.716mmol)} were suspended in acetone (1.5cm3) and then added individually to alkaline mixtures comprised of NaOH (0.0286g, 0.716mmol) in distilled water (1cm3). Upon dissolution of the organic precursors, the corresponding solutions were introduce in a dropwise manner to particular reaction mixtures of di(2-picolyl)amine (0.1001g, 0.5024mmol) and K2CO3 (0.069g, 0.5018mmol) in acetone (4.0cm3). Thereafter, the resultant reaction mixtures were heated at reflux for 24h, which was followed by the reduction of the solvent under vacuum. The respective residues were dispersed in separate 1:1 (v:v) water and chloroform combinations. Then the crude individual oily products were attained by the triplicate extractions from the aqueous mixture using chloroform and these extracts were dried over anhydrous MgSO4 prior to removing the solvent under reduced pressure. The relating crude products were purified by column chromatography using a silica stationary phase and DCM: MeOH (v:v, 9:1) as a mobile phase. 2.2.2 6-((bis(pyridin-2-ylmethyl)amino)methyl)uracil (Hurdpa) X-ray quality single crystals were grown via the slow diffusion of n-hexane into a solution of dichloromethane. Yield: 0.72g (51%). Molecular mass (m/z): Cald. for C17H17N5O2: 323.14. Found: 346.13 [M+Na]+ (Fig. S3). FTIR (cm-1): v(N-H) 3370 (br, w); v(C=O) 1681 (vs); v(C=N) 1579 (s); v(C-N) 1161, 1136 (m). 1H NMR (d6-DMSO/ppm/298K, Fig. S4): 11.04 (br, s, 1H, N5H); 10.87 (s, 1H, N4H); 8.55-8.50 (m, 2H, H1, H12); 7.84-7.75 (m, 2H, H3, H10); 7.52-7.46 (m, 2H, H2, H11); 7.33-7.24 (m, 2H, H4, H9); 5.57 (s, 1H, H17); 3.90-3.83 (m, 4H, H6, H6?, H7, H7?); 3.52 (br, s, 2H, H13, H13?). UV-Vis (MeOH, lambdamax (epsilon, M-1cm-1)): 256nm (sh, 1540); 262nm (1720); 268nm (sh, 1350); 359nm (10)

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 18592-13-7, 6-(Chloromethyl)pyrimidine-2,4(1H,3H)-dione.

Reference:
Article; Gramni, Larusha; Vukea, Nyeleti; Chakraborty, Abir; Samson, William John; Dingle, Laura Margaret Kirkpartick; Xulu, Bheki; de la Mare, Jo-Anne; Edkins, Adrienne Lesley; Booysen, Irvin Noel; Inorganica Chimica Acta; vol. 492; (2019); p. 98 – 107;,
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Analyzing the synthesis route of Synthetic Route of 2227-98-7

According to the analysis of related databases, 2227-98-7, the application of this compound in the production field has become more and more popular.

Synthetic Route of 2227-98-7, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 2227-98-7, name is 4-Aminopyrrolo[3,2-d]pyrimidine. This compound has unique chemical properties. The synthetic route is as follows.

Example 17.4: (3f?,4S)-4-Butyl-1-[(9-deaza-adenin-9-yl)methyl]-3-hydroxypyrrolidine (20, R = Et); Formaldehyde (86 mul_, 1.1 mmol, 37 wt% solution in water) followed by 9-deazaadenine (112 mg, 0.84 mmol) are added to a solution of 19 (R = Et) (100 mg, 0.56 mmol) in 1 ,4-dioxane (1 mL) and water (2 ml_). The reaction mixture is warmed to 85 0C and after 1 h the crude reaction mixture absorbed onto silica and eluted down a silica column using a gradient 5 – 30% (7 N NH3 in MeOH) in CH2CI2. The crude product is collected, concentrated and subjected to flash chromatography (5 : 4.5 : 0.5, CH2CI2 : MeOH : 28% aq. NH4OH) to afford 20 (R = Et) as an off- white solid (90 mg, 56%). 1H NMR (500 MHz, CD3OD): delta = 8.17 (s, 1H), 7.49 (s, 1H), 3.86 – 3.83 (m, 1 H), 3.81 (q, J = 13.2 Hz, 2H), 3.05 (dd, J = 9.6, 8.0 Hz, 1H), 2.74 (dd, J = 10.4, 6.3 Hz, 1 H), 2.69 (dd, J = 10.4, 4.0 Hz, 1H), 2.17 (dd, J = 9.7, 8.0 Hz. 1H), 1.98 – 1.90 (m, 1H), 1.57 – 1.47 (m, 1H), 1.34 – 1.24 (m, 5H) and 0.89 ppm (t, J = 6.9 Hz, 3H). 13C NMR (125 MHz, CD3OD): delta = 152.1 , 151.0, 147.0, 130.1 , 115.1, 112.6, 77.8, 62.4, 59.7, 49.1 , 48.6, 34.0, 31.5, 23.8 and 14.4 ppm. ESI-HRMS for C15H24N5O [MH]+ calcd, 290.1981; found, 290.1988

According to the analysis of related databases, 2227-98-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ALBERT EINSTEIN COLLEGE OF YESHIVA UNIVERSITY; INDUSTRIAL RESEARCH LIMITED; EVANS, Gary Brian; LONGSHAW, Alistair Ian; SCHRAMM, Vern L.; TYLER, Peter, Charles; WO2011/8110; (2011); A1;,
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Simple exploration of Computed Properties of C4H2ClFN2O

With the rapid development of chemical substances, we look forward to future research findings about 155-12-4.

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 155-12-4, name is 2-Chloro-5-fluoropyrimidin-4-one, molecular formula is C4H2ClFN2O, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. Computed Properties of C4H2ClFN2O

Example 1b 2-(2-Chloro-5-fluoro-6-oxo-6H-pyrimidin-1-ylmethyl)-benzonitrile The title compound was prepared in 44% yield from 2-chloro-5-fluoro-3H-pyrimidin-4-one as described in U.S. patent application Ser. No. 10/918,317. Specifically, 5-Fluoro-2-chloro-3H-pyrimidin-4-one was stirred in DME/DMF under nitrogen at 0 C. Sodium hydride (95%) was added in portions. After 10 min, lithium bromide was added and the reaction stirred at r.t. alpha-Bromo-o-tolunitrile was added, and the reaction stirred at 65 C. for 8 h. The solution was diluted with EtOAc, washed with brine, dried (MgSO4) and concentrated in vacuo. Purification by silica gel chromatography (1:1:1 EtOAc/hexanes/CHCl3) gave the title compound. Also obtained from the reaction were impure fractions of the less polar O-alkylated isomer, and the more polar N3-alkylated isomer. 1H NMR (400 MHz, CDCl3): delta 7.81 (s, 1H), 7.74 (dd, 1H, J=7.6, 1.2 Hz), 7.59 (td, 1H, J=7.6, 1.2 Hz), 7.45 (t, 1H, J=7.6 Hz), 7.15 (d, 1H, J=7.6 Hz), 5.67 (s, 2H). MS (ES) [m+H] calc’d for C12H7N3OFCl, 264, 266; found 264, 266.

With the rapid development of chemical substances, we look forward to future research findings about 155-12-4.

Reference:
Patent; Chyall, Leonard J.; Lorimer, Keith; McClausland, Linda J.; US2007/66636; (2007); A1;,
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