Day: January 15, 2021

Adding a certain compound to certain chemical reactions, such as: 6297-80-9, 4,6-Dichloropyrimidin-2(1H)-one, 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 4,6-Dichloropyrimidin-2(1H)-one, blongs to pyrimidines compound. Quality Control of 4,6-Dichloropyrimidin-2(1H)-one

General procedure: #10;4,6-dichloropyrimidin-2(1H)-one (0.24 mmol) and the amine (0.24 mmol) was dissolved in NMP (1 ml) in a microwave vial. The vial was capped and heated at 120 ¡ãC for 15 min in a single node microwave reactor. Morpholine (7.5 mmol) was added and the mixture was heated at 120 ¡ãC for 30 min. The reaction mixture was worked up with DCM (3 ml) and brine (1 ml) and filtered through a phase separator. The compound was purified with HPLC using FractionLynx I instrument, Mobilphase: gradient 5-95percent ACN in 0.1 M HCO2H, pH3, Column: Sunfire Prep C18 5m OBD 19*150 mm to give the product.

The synthetic route of 6297-80-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Giordanetto, Fabrizio; Wallberg, Andreas; Ghosal, Saswati; Iliefski, Tommy; Cassel, Johan; Yuan, Zhong-Qing; Von Wachenfeldt, Henrik; Andersen, Soren M.; Inghardt, Tord; Tunek, Anders; Nylander, Sven; Bioorganic and medicinal chemistry letters; vol. 22; 21; (2012); p. 6671 – 6676,6;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Application of 3993-78-0, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 3993-78-0 as follows.

2-Amino-4-chloropyrimidine (55) (13.0g, 100mmol) was added to a 57wt.% aqueous solution of hydriodic acid (115ml, 1.00mol) at 0C and the mixture was stirred at room temperature for 3h. The mixture was cooled to 0C and the resulting precipitate was removed by filtration and taken up in cold 5N aqueous Na2CO3 (200ml). The mixture was extracted with EtOAc (3¡Á500ml) and the combined organic layers were concentrated under reduced pressure to deliver 2-amino-4-iodopyrimidine (21.1g, 95.0mmol, 95% yield) as a white solid. 1H NMR (400MHz, DMSO-d6) delta ppm 7.78 (d, J=5.0Hz, 1H), 7.02 (br. s, 2H), 7.00 (d, J=5.0Hz, 1H). MS (ESI, pos. ion) m/z: 222.1 (M+1).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,3993-78-0, its application will become more common.

Reference:
Article; Reichelt, Andreas; Bailis, Julie M.; Bartberger, Michael D.; Yao, Guomin; Shu, Hong; Kaller, Matthew R.; Allen, John G.; Weidner, Margaret F.; Keegan, Kathleen S.; Dao, Jennifer H.; European Journal of Medicinal Chemistry; vol. 80; (2014); p. 364 – 382;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Adding a certain compound to certain chemical reactions, such as: 183438-24-6, 5-Bromo-2-iodopyrimidine, 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, 183438-24-6, blongs to pyrimidines compound. Recommanded Product: 183438-24-6

INTERMEDIATE 163 -(5 -Bromopyrimidin-2-yl)-3 -hydroxycyclobutyl 2,2-dimethylpropanoate5-Bromo-2-iodopyrimidine (16.7 g, 58.8 mmol) was dissolved in DCM (200 mL) with stirring and cooled to -78C under N2. n-Butyllithium in hexane (2.5M, 23.5 mL)was added dropwise and the mixture was stirred for 20 minutes at -78C. Intermediate 15 (10 g, 58.8 mmol) in DCM (50 mL) was cooled in a dry ice bath and added in one portion. The reaction mixture was stirred at -78C for 10 minutes, then quenched by the addition of saturated aqueous NH4C1 solution (20 mL) and allowed to warm to room temperature. Saturated aqueous NH4C1 solution (50 mL) was added and the mixture wasextracted with DCM (2 x 100 mL). The combined organic extracts were dried over sodium sulfate and concentrated in vacuo. The crude residue was purified by column chromatography (5i02, 0-30% EtOAc in heptane), yielding the title compound (7.6 g, 35%) as a yellow solid. H (500 MHz, CDC13) 8.78 (s, 2H), 5.22-5.14 (m, 1H), 3.03-2.93 (m, 2H), 2.67-2.58 (m, 2H), 1.22 (s, 9H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,183438-24-6, its application will become more common.

Reference:
Patent; UCB BIOPHARMA SPRL; DELIGNY, Michael Louis Robert; HEER, Jag Paul; JACKSON, Victoria Elizabeth; KROEPLIEN, Boris; LECOMTE, Fabien Claude; PORTER, John Robert; WO2015/86509; (2015); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Related Products of 53112-28-0, 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. 53112-28-0, name is 4,6-Dimethyl-N-phenyl-2-pyrimidinamine. A new synthetic method of this compound is introduced below.

Preparation of the Co-Crystal Comprising Pyrimethanil and Dithiine Tetracarboximide of the Formula (I). Preparation 83 mg of pyrimethanil and 117 mg of dithiine tetracarboximide of the formula (I) are suspended in 2 mL of water or in a mixture of water and polar organic solvent. The suspension solution is stirred until a red powder is obtained (pyrimethanil is a white powder, dithiine tetracarboximide of the formula (I) is a blue powder). The solid material is separated by filtration and dried at 25 C. for 12 hours. The corresponding PXRD pattern and DSC trace are shown in FIG. 1 and in FIG. 3, respectively.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,53112-28-0, its application will become more common.

Reference:
Patent; BASF SE; BRATZ, Matthias; CHIODO, Tiziana; KOULELIS, Dennis; MERTOGLU, Murat; (16 pag.)US2016/15034; (2016); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Electric Literature of 63931-21-5 ,Some common heterocyclic compound, 63931-21-5, molecular formula is C4BrCl3N2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.

5-Bromo-2,4,6-trichloropyrimidine (1.880 g, 6.81 mmol) was dissolved in THF (11 mL) and water (5 mL), and sodium acetate (1.68 g, 20.4 mmol), followed by 4-fluoroaniline (787 mg, 0.68 mL, 6.87 mmol) were added. The mixture was stirred at room temperature for 18 h. After that, a saturated aqueous solution of sodium hydrogencarbonate (15 mL) was added and the resulting mixture was extracted with ethyl acetate (2 x 150 mL). The combined organic layers were dried (sodium sulfate) and concentrated in vacuo. The crude was purified by column chromatography (silica gel, 40 g, eluting with ethyl acetate / n-heptane, gradient 0: 100 to 10:90) to afford, after drying in vacuo (40C, 5 mbar), the title compound as a light brown solid (2.07 g, 90%). HPLC (method LCMS_fastgradient) tR = 1.36 min. 1H NMR (CDC13, 300 MHz): delta 7.12 (dd, / = 8.3, 9.1 Hz, 2 H), 7.43 (br s, 1 H), 7.52 (dd, / = 4.6, 8.9 Hz, 2 H). MS (ES+) m/z 335.9, 337.9, 339.9 [M+H, Br & 2 CI isotopes] .

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,63931-21-5, its application will become more common.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; BARTELS, Bjoern; JAKOB-ROETNE, Roland; LIMBERG, Anja; NEIDHART, Werner; RATNI, Hasane; REUTLINGER, Michael; STEINER, Sandra; (89 pag.)WO2018/11164; (2018); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Synthetic Route of 16019-33-3, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 16019-33-3 as follows.

Step 1 : 7-(4-Bromo-3-fluorophenyl)-4-chloro-6,7-dihydro-5H-pyrrolo[2,3- c/]pyrimidine (141) A round bottom flask was charged with 4-bromo-3-fluoroaniline (10.0 g, 52.5 mmol) and then cooled to -150C. Trifluoroacetic acid (50 ml.) was added to the above cold aniline while stirring the contents for 0.5 h. Na(OAc)3BH (15.9 g, 50 mmol) was added portion wise to the above mixture and stirred for additional 0.5 h. The aldehyde 209 (see example 118, step 1 , 7.85 g, 75 mmol) in CH2CI2 (15 ml.) was added to the above mixture. The resultant mixture was allowed to warm up to the ambient temperature and stirred for 24 h. The reaction mixture was concentrated under reduced pressure and the residue was poured into sat. NaHCO3 solution (250 ml.) and then the mixture was extracted with CH2CI2 (3 x 250 ml_). The combined organic layer was washed with brine (1 x 100 ml_), dried over sat. Na2SO4 and then concentrated under reduced pressure to afford crude material, which was recrystallized from CH2CI2 and MeOH to afford 8.65 g (53%) of the title prodcuct 141_as an off-white solid. 1H NMR (400 MHz, DMSO-c/6): delta 8.42 (s, 1 H), 7.88 and 7.86 (dd, J1 = 11.2 Hz, J2 = 2.8 Hz, 2 H), 7.51 (t, J = 8.0 Hz, 1 H), 7.36 and 7.34 (dd, J1 = 9.2 Hz, J2 = 2.4 Hz, 1 H), 4.11 (t, J = 8.8 Hz, 2 H), 3.22 (t, J = 8.4 Hz, 2 H); LCMS (ESI): m/z 329 (M + H)+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,16019-33-3, its application will become more common.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2008/8895; (2008); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Related Products of 6299-25-8 ,Some common heterocyclic compound, 6299-25-8, molecular formula is C5H4Cl2N2S, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.

4,6-dichloro-2-(methylthio)pyrimidine (0.7?g, 3.608?mmol) was dissolved in dichloromethane (15?mL), cooled to 0?C and meta-Chloroperoxybenzoic acid (m-CPBA) was added (1.55?g, 9.011?mmol) portion wise to the reaction mixture at the same temperature. After addition, the reaction mixture was allowed to stir for 4?h at room temperature. Then the reaction mass was quenched with an aqueous solution of sodium thiosulphate (11?mL) and extracted with dichloromethane (2?*?10?mL). Combined organic layer was washed with saturated aqueous NaHCO3 solution (15?mL), brine solution (7?mL), dried over anhydrous MgSO4, filtered and the filtrate was evaporated under reduced pressure to afford 4,6-dichloro-2-(methylsulfonyl)pyrimidine (0.65?g, 80.20%) as off-white solid ( Scheme -1).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 6299-25-8, 4,6-Dichloro-2-(methylthio)pyrimidine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Murthy, P. Krishna; Valverde, Clodoaldo; Suneetha; Armakovi?, Stevan; Armakovi?, Sanja J.; Rani, N. Usha; Naidu, N. Venkatasubba; Journal of Molecular Structure; vol. 1186; (2019); p. 263 – 275;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Synthetic Route of 98136-42-6, 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 98136-42-6, name is 2,6-Dichloropyrimidine-4-carboxamide. This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 2,6-dichloropyrimidine-4-carboxamide (0.385 g, 2.01 mmol) in THF (10 mL) was added (S)-ethyl 2-hydroxypropanoate (0.26 mL, 2.3 mmol). The mixture was cooled on a dry-ice acetone bath and 60% NaH in mineral oil (0.094 g, 2.4 mmol) was added. The reaction was allowed to warm up slowly and after 2 h was quenched with 2 mL 10% citric acid solution. The reaction mixture was partitioned between 50 mL EtOAc and 25 mL brine and the organic fraction dried over MgSO4, filtered and concentrated in vacuo. The residue was dissolved in dioxane (10 mL) and 2-(4-(4-fluorophenoxy)phenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (0.691 g, 2.20 mmol), 2M aqueous Na2CO3 (2.0 mL, 4.0 mmol), and PdCl2(dppf) (0.091 g, 0.1 1 mmol) were added. The reaction vessel was flushed with argon, sealed, and heated at 100C overnight. After cooling, the reaction mixture was evaporated in vacuo and the residue chromatographed over silica gel with 10-50% acetone in hexanes. The product fractions were evaporated in vacuo to give (S)-ethyl 2-((6-carbamoyl-2-(4-(4-fluorophenoxy)phenyl)pyrimidin-4-yl)oxy)propanoate as a pale tan oil (0.762 g, 1.79 mmol, 90% yield).

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 98136-42-6, 2,6-Dichloropyrimidine-4-carboxamide.

Reference:
Patent; PURDUE PHARMA L.P.; LOCKMAN, Jeffrey; NI, Chiyou; PARK, Jae Hyun; PARK, Minnie; SHAO, Bin; TAFESSE, Laykea; YAO, Jiangchao; YOUNGMAN, Mark, A.; WO2014/135955; (2014); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Synthetic Route of 289042-12-2, 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. 289042-12-2, name is tert-Butyl 2-((4R,6S)-6-((E)-2-(4-(4-fluorophenyl)-6-isopropyl-2-(N-methylmethylsulfonamido)pyrimidin-5-yl)vinyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate. A new synthetic method of this compound is introduced below.

The method for synthesizing the rosuvastatin calcium chiral isomer impurity of the present embodiment comprises the following steps:(1) 20g compound I was added to 500mL three reaction flask, stirred and dissolved in 220mL of acetonitrile was added dropwise 60mL 0.05M hydrochloric acid, the reaction was incubated dropwise at 35 ~ 40 C for 3 hours until the starting material disappeared (TLC: Ester: petroleum ether = 6: 1),The pH was adjusted to neutral with 5% sodium bicarbonate solution, the acetonitrile was removed by distillation under reduced pressure, extracted twice with methylene chloride (100 mL * 2), dried over anhydrous sodium sulfate, filtered,The filtrate was transferred to 500mL three reaction flask, 60g of manganese dioxide was added, the reaction was refluxed for 20 hours, the reaction was over, filtered, the filtrate was evaporated under reduced pressure and concentrated to dryness to give 17.6g light yellow oil, namely compound III, directly into the next reaction; The yield of compound III was 95.2%

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,289042-12-2, its application will become more common.

Reference:
Patent; Zhejiang Mei Nuohua Pharmaceutical Chemical Co., Ltd.; Yu Kui; Huang Xiangliang; Jia Jiangnan; Liu Tao; Yu Shenggang; Lin Zufeng; Chen Weiren; Yao Chengzhi; (12 pag.)CN107382875; (2017); A;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Electric Literature of 50593-92-5, Adding some certain compound to certain chemical reactions, such as: 50593-92-5, name is 5-Bromo-2-(methylthio)pyrimidine-4-carboxylic acid,molecular formula is C6H5BrN2O2S, 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 50593-92-5.

(b). 2-Methylsulfanyl-pyrimidine-4-carboxylic acid; The product of example 21a (517 mg) in methanol (25 ml) was hydrogenated in a PARR apparatus in the presence of KOH (260 mg) and 10% Pd on BaSO4 (260 mg) for4 h. The reaction mixture was filtered over decalite and washed with methanol (warm), The filtrate was concentrated to 50% of its volume followed by addition of cone. HCl(33%) to pH 1. The precipitate (KBr) was filtered off and the mother liquor was concentrated in vacuo. The residue was recrystallized from dioxane. Yield: 200 mg. MS-ESI: [M+H]+ = 170

According to the analysis of related databases, 50593-92-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; N.V. ORGANON; WO2006/117368; (2006); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia