Category: 696-07-1

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 696-07-1, name is 5-Iodouracil. This compound has unique chemical properties. The synthetic route is as follows. category: pyrimidines

5-bromo- or 5-iodouracil (1.0 equiv.) is suspended in N,N-dimethylaniline, treated with phosphorus oxychloride (10.0 equiv.) and stirred for 90 minutes at 125 C. After cooling to room temperature, excess phosphorus oxychloride is removed under vacuum. The residue is poured into ice-water. After 2 hours the crystals that have formed are filtered off at the pump and washed with water. Next, the crystals are dissolved in ethyl acetate. The organic phase is washed with saturated sodium hydrogen carbonate solution and saturated sodium sulphite solution and dried over sodium sulphate. After removal of the solvent the chromatographic purification is performed.; Starting from 5-iodouracil (10g, 42 mmol)) and N,N-dimethylaniline (11.0 mL), the desired product is obtained according to procedure 1 in 92% yield (10.6 g) after chromatographic purification (silica gel, dichloromethane). 1H-NMR (400 MHz, CDCl3): delta 8.90 (s, 1H).

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, 696-07-1, 5-Iodouracil.

Reference:
Patent; Lucking, Ulrich; Nguyen, Duy; Von Bonin, Arne; Von Ahsen, Oliver; Kruger, Martin; Briem, Hans; Kettschau, Georg; Prien, Olaf; Mengel, Anne; Konrad, Krolikiewicz; Boemer, Ulf; Bothe, Ulrich; Hartung, Ingo; US2007/232632; (2007); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Adding a certain compound to certain chemical reactions, such as: 696-07-1, 5-Iodouracil, 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, HPLC of Formula: C4H3IN2O2, blongs to pyrimidines compound. HPLC of Formula: C4H3IN2O2

General procedure: In a typical experiment Pd(OAc)2, triphenylphosphine, iodouracil derivatives (1, 5), amine nucleophiles (a-g) and triethylamine were used in the same amount as above and were dissolved in 10mL of DMF under argon in a 100mL autoclave. The atmosphere was changed to carbon dioxide and the autoclave was pressurized to the given pressure with carbon monoxide. (Caution: High pressure carbon monoxide should only be used with adequate ventilation (hood) using CO sensors as well.) The reaction was conducted for the given reaction time upon stirring at 50C. After the given reaction time the reaction mixture was cooled to room temperature and the autoclave was carefully depressurized in a well-ventilated hood. The product mixture was analysed by GC and GC-MS. The work-up of the reaction mixture was identical to that discussed for the atmospheric experiments. 3.4.1 5-(N-tert-Butylglyoxylamido)uracil (3a) Yield: 175mg (73%), Off white powder, m.p. 270-271C; Rf (15% MeOH/CHCl3) 0.65. deltaH (500MHz, DMSO-d6) 11.82 (1H, br s, NH), 11.42 (1H, br s, NH), 8.20 (1H, s, NHCH), 7.98 (1H, s, CONH), 1.31 (9H, 3 x (CH)3). deltaC NMR (125.7MHz) 186.6, 165.7, 161.3, 150.9, 150.6, 108.8, 51.1, 28.7. IR (KBr, nu (cm-1)): 3375 (NH), 1734, 1700, 1669 (CO), 1653 (Amide I.), 1616 (C=C), 1499 (Amide II.); MS m/z (rel. int.): 238 (100, [M-H]-), MS/MS (rel. int.) 238 (19), 223 (10), 195 (32), 123 (8), 111 (100).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,696-07-1, 5-Iodouracil, and friends who are interested can also refer to it.

Reference:
Article; Kollar, Laszlo; Varga, Marta Georgina; Doernyei, Agnes; Takacs, Attila; Tetrahedron; vol. 75; 33; (2019); p. 4632 – 4639;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

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.696-07-1, name is 5-Iodouracil, molecular formula is C4H3IN2O2, molecular weight is 237.9833, as common compound, the synthetic route is as follows.Safety of 5-Iodouracil

To a dry DMF (50 mL) solution of 5-iodouracil 23 (5.00 g, 21 mmol), tetrakis (triphenylphosphine) palladium (0) (1.00 g, 0.87 mmol, 0.04 equiv. ) and copper iodide (0.80 g, 4.2 mmol, 0.2 equiv. ) under a nitrogen atmosphere was added dry DIPEA (7.3 mL, 5.42 g, 42 mmol, 2 equiv. ) and 1-DODECYNE 24 (13.5 ML, 10.48 g, 63 mmol, 3 equiv. ) via syringe with stirring. The initially opaque yellow solution proceeded to change colour on stirring at room temperature to a clear dark yellow solution, and eventually an opaque dark green suspension formed after a couple of hours. The suspension was allowed to react at RT with stirring for 18 h. TLC analysis of the resulting mixture indicated that most of the starting material had reacted, and the presence of a blue fluorescent spot was clearly observed. Dry triethylamine (25 mL) and a further addition of copper iodide (0.80 g) was then made to the suspension, and the resultant reaction mixture heated to 80 C for 6 h with stirring under N2. The suspension was allowed to cool to RT overnight with stirring. The resultant precipitate was collected by suction filtration, and washed consecutively with methanol and DCM. The collected solid was triturated in hot methanol to yield the title COMPOUND 26 as a white insoluble solid of weight 3.79 g (65 % from 23).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,696-07-1, 5-Iodouracil, and friends who are interested can also refer to it.

Reference:
Patent; UNIVERSITY COLLEGE CARDIFF CONSULTANTS LIMITED; REGA FOUNDATION; WO2004/96813; (2004); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Synthetic Route of 696-07-1, Adding some certain compound to certain chemical reactions, such as: 696-07-1, name is 5-Iodouracil,molecular formula is C4H3IN2O2, 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 696-07-1.

5-Iodouracil (23.8 g), TEA (30.3 g), Tol (240 mL) were placed in a 500 mL three-necked flask and heated to 100 C.When the internal temperature of the bottle reached 90 C, phosphorus oxychloride (33.7 g) was slowly added dropwise.After the addition was completed, the temperature was kept stirring for 1 h, then cooled to room temperature, suction filtered, and the filtrate was collected.The solid was washed with PE/EA=5/1, and the filtrate and washing solution were combined.Spin dry to obtain a crude product and then beat with PE to give the product 24.5 g of an off-white solid.The yield was 89%.

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. 696-07-1, 5-Iodouracil, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Beijing Ruiboao Biological Technology Co., Ltd.; Liu Zhiqiang; Li Yazhou; Chen Zhenchang; Zhang Hongjuan; (7 pag.)CN109761914; (2019); A;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Reference of 696-07-1, 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 696-07-1, name is 5-Iodouracil. This compound has unique chemical properties. The synthetic route is as follows.

A. Preparation of 5-iodo-2,4-dioxo-3,4-dihydro-2H-pyrimidine-l-carboxylic acid tert-butyl ester; A 500 ml single neck round bottom flask was charged with 5-iodouracil (5.0g, 21mmol) and dry acetonitrile (200ml). Dimethyl amino pyridine (26mg, 0.21mmol) was added in one portion followed by drop wise addition of di-t-butyl di carbonate (5.5g, 25.2mmol) at room temperature and stirred for 3h at room temperature. The reaction mixture was filtered and the organic layer was concentrated under vacuum. Yield = 7.1 (100%)The proton NMR data of the desired product, 5-iodo-2,4-dioxo-3,4-dihydro-2H- pyrimidine-1 -carboxylic acid tert-butyl ester, is provided below: 1H NMR (400 MHz, DMSO-d6, deltappm):CH3)

According to the analysis of related databases, 696-07-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JUBILANT BIOSYS LIMITED; WO2007/122634; (2007); A2;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 696-07-1, name is 5-Iodouracil, the common compound, a new synthetic route is introduced below. COA of Formula: C4H3IN2O2

A suspension of 5-iodouracil (1.8g, 7.54mmol) in dry acetonitrile (15mL) was treated with N,O-bis(trimethylsilyl) acetamide (4.62mL, 18.87mmol) and left to stir until the solution became clear. A solution of a mixture of isoxazolidines 12, 13 (2.6g, 6.29mmol) in dry acetonitrile (15mL) and trimethylsilyl triflate (0.22mL, 1.25mmol) was then added, and the reaction mixture was stirred at room temperature overnight. After this time, the solution was carefully neutralized by the addition of 5% aqueous sodium hydrogen carbonate and then concentrated in vacuo. After addition of dichloromethane (20mL), the organic phase was separated, washed with water (2×10mL), dried with sodium sulfate, filtered, and concentrated. The 1H NMR spectrum of the crude reaction mixture showed the presence of beta-anomers (cis) as nearly exclusive adducts, whereas the alpha-anomers were present only in trace amounts. The residue was purified by MPLC on a silica gel column (cyclohexane/ethyl acetate, 7:3) to afford 14. Yellow oil, 3.65g, 90% yield. 1H NMR (500MHz, CDCl3): delta=8.90 (br s, 1H), 8.25 (s, 1H), 7.65 (dd, J=7.9, 1.4Hz, 4H), 7.49-7.37 (m, 6H), 6.01 (dd, J=7.5, 3.4Hz, 1H), 3.71 (dd, J=4.7, 2.0Hz, 2H), 2.96 (dt, J=13.7, 7.8Hz, 2H), 2.90-2.84 (m, 1H), 2.82 (s, 3H), 2.25-2.09 (m, 1H), 1.05 (s, 9H). 13C NMR (126MHz, CDCl3): delta=160.23, 150.15, 145.33, 135.69, 132.83, 130.10, 128.02, 83.84, 69.35, 67.65, 63.08, 44.85, 41.82, 26.95, 19.31. Anal. calcd for C25H30IN3O4Si: C, 50.76; H, 5.11; N, 7.10; found: C, 50.73; H, 5.12; N, 7.11.

The synthetic route of 696-07-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Romeo, Roberto; Giofre, Salvatore V.; Garozzo, Adriana; Bisignano, Benedetta; Corsaro, Antonino; Chiacchio, Maria A.; Bioorganic and Medicinal Chemistry; vol. 21; 18; (2013); p. 5688 – 5693;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Electric Literature of 696-07-1, 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 696-07-1 as follows.

5-Iodouracil (0.10 g, 0.42 mmol) was suspended in dry MeCN (2.1 mL) and N,O-bis(trimethylsilyl)acetamide (0.25 mL, 1.05 mmol) was added under nitrogen atmosphere. When the reaction mixture turned clear, bromodiphenyl methane (0.15 g, 0.63 mmol) and a catalytic amount of I2 were added and the reaction mixture was heated at 84 C. for 4 hrs. After cooling to room temperature, the mixture was concentrated under reduced pressure, diluted with EtOAc and washed with water. The aqueous phase was extracted with EtOAc (3*15 mL), the combined organic layers were washed with brine, dried over Na2SO4 and the solvent was removed under reduced pressure. The crude was purified by column chromatography using a Teledyne ISCO apparatus (cyclohexane:EtOAc 60:40) to afford the title compound (0.15 g, 87%) as white solid. 1H NMR (400 MHz, CDCl3): delta 7.02 (s, 1H), 7.14-7.18 (m, 4H), 7.38-7.45 (m, 6H), 7.46 (s, 1H), 8.58 (s, 1H). MS (ESI) in/Z: 405 [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,696-07-1, its application will become more common.

Reference:
Patent; Piomelli, Daniele; Realini, Natalia; Mor, Marco; Pagliuca, Chiara; Pizzirani, Daniela; Scarpelli, Rita; Bandiera, Tiziano; US2015/111892; (2015); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Application of 696-07-1 ,Some common heterocyclic compound, 696-07-1, molecular formula is C4H3IN2O2, 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-Iodouracil (23.8 g), TEA (30.3 g), Tol (240 mL) were placed in a 500 mL three-necked flask and heated to 100 C.When the internal temperature of the bottle reached 90 C, phosphorus oxychloride (33.7 g) was slowly added dropwise.After the addition was completed, the temperature was kept stirring for 1 h, then cooled to room temperature, suction filtered, and the filtrate was collected.The solid was washed with PE/EA=5/1, and the filtrate and washing solution were combined.Spin dry to obtain a crude product and then beat with PE to give the product 24.5 g of an off-white solid.The yield was 89%.

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. 696-07-1, 5-Iodouracil, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Beijing Ruiboao Biological Technology Co., Ltd.; Liu Zhiqiang; Li Yazhou; Chen Zhenchang; Zhang Hongjuan; (7 pag.)CN109761914; (2019); A;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Synthetic Route of 696-07-1, 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 696-07-1 as follows.

Step 1 . Preparation of 1 -benzhydryl-5-iodo-pyrimidine-2,4-dione 5-lodouracil (0.10 g, 0.42 mmol) was suspended in dry MeCN (2.1 mL) and Nu, Omicron- bis(trimethylsilyl)acetamide (0.25 mL, 1 .05 mmol) was added under nitrogen atmosphere. When the reaction mixture turned clear, bromodiphenyl methane (0.15 g, 0.63 mmol) and a catalytic amount of l2 were added and the reaction mixture was heated at 84 C for 4 hrs. After cooling to room temperature, the mixture was concentrated under reduced pressure, diluted with EtOAc and washed with water. The aqueous phase was extracted with EtOAc (3 x 15 mL), the combined organic layers were washed with brine, dried over Na2SO4 and the solvent was removed under reduced pressure. The crude was purified by column chromatography using a Teledyne ISCO apparatus (cyclohexane:EtOAc 60:40) to afford the title compound (0.15 g, 87%) as white solid. 1H NMR (400 MHz, CDCI3): delta 7.02 (s, 1 H), 7.14-7.18 (m, 4H), 7.38-7.45 (m, 6H), 7.46 (s, 1 H), 8.58 (s, 1 H). MS (ESI) m/z: 405 [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,696-07-1, its application will become more common.

Reference:
Patent; FONDAZIONE ISTITUTO ITALIANO DI TECNOLOGIA; THE REGENTS OF THE UNIVERSITY OF CALIFORNIA; UNIVERSITA’ DEGLI STUDI DI PARMA; PIOMELLI, Daniele; REALINI, Natalia; MOR, Marco; PAGLIUCA, Chiara; PIZZIRANI, Daniela; SCARPELLI, Rita; BANDIERA, Tiziano; WO2013/178576; (2013); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Synthetic Route of 696-07-1, Adding some certain compound to certain chemical reactions, such as: 696-07-1, name is 5-Iodouracil,molecular formula is C4H3IN2O2, 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 696-07-1.

General procedure: To a solution of 5-iodopyrimidine (0.84 mmol) in anhydrous DMF (7 mL) were added the terminal alkyne (2.5 mmol), Pd(PPh3)4 (0.08 mmol), CuI (0.08 mmol) and Et3N [or (iPr)2EtN] (1.68 mmol). Method A: The reaction mixture was stirred at room temperature overnight. The extent of the reaction was monitored by TLC and the solvent was evaporated in vacuo and the residue purified by column chromatography (initial eluent CH2Cl2, then CH2Cl2/MeOH = 40:1) to afford 1-10a and 1-6b. Method B: The synthesis was carried out at 50 C for 30 min under microwave irradiation (300 W, 1 bar, Milestone start S microwave oven). Purification by column chromatography (initial eluent CH2Cl2, then CH2Cl2/MeOH = 40:1) afforded compounds 1-10a and 1-6b.

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. 696-07-1, 5-Iodouracil, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Kraljevi?, Tatjana Gazivoda; Bistrovi?, Andrea; Dedi?, Matea; Paveli?, Sandra Kraljevi?; Sedi?, Mirela; Rai?-Mali?, Silvana; Tetrahedron Letters; vol. 53; 38; (2012); p. 5144 – 5147;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia