Category: 33252-64-1

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. 33252-64-1, name is 3-Nitro-5-(trifluoromethyl)pyridin-2(1H)-one. A new synthetic method of this compound is introduced below., Application In Synthesis of 3-Nitro-5-(trifluoromethyl)pyridin-2(1H)-one

2-Hydroxy-3-nitro-5-trifluoromethylpyridine (8.8 g, 42.3 mmol) was added to a mixture of phosphorous oxychloride (4.2 mL, 45.9 mmol) and phosphorous pentachloride (9.6 g, 46.1 mmol) at 60 C. The reaction mixture was then heated under nitrogen at 80 C. overnight. The resulting dark product mixture was allowed to cool to room temperature and was poured into ice/water. The mixture was extracted with ether and the ether extract was washed with water and brine. After drying over magnesium sulfate, the solvent was removed to leave a dark oil which was subjected to flash chromatography on silica gel eluding with chloroform. Fractions containing only the desired product were combined and concentrated to leave a brown oil (5.0 g, 52%). 1 H NMR (DMSO-d6): delta9.20 (s, 1H), 9.07 (s, 1H).

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Reference:
Patent; Pfizer Inc; US5811432; (1998); A;,
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Pyridine | C5H5N – PubChem

Synthetic Route of 33252-64-1, 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. 33252-64-1, name is 3-Nitro-5-(trifluoromethyl)pyridin-2(1H)-one. A new synthetic method of this compound is introduced below.

3-Nitro-5-(trifluoromethyl)pyridin-2-ol (31.00 g, 149 mmol) was dissolved in acetonitrile (250 ml) to give a dark brown solution. Phosphorus(V) oxybromide (85 g, 298 mmol) was added and the mixture was heated at reflux for 4 hours and then stirred at RT overnight. The reaction mixture was quenched by pouring into vigorously stirring water (600 ml) containing sodium hydrogencarbonate (1 10 g). The dark brown mixture was extracted with DCM (3 x 200 ml) and the organic phase was washed with water (200 ml) and brine (100ml), dried (MgS04) and concentrated under reduced pressure to afford the title product as a brown oil. H-NMR: [400MHz, CDCI3, ? 8.87 (1 H, d, J = 1.4Hz, ArH), 8.39 (1 H, d, J = 1 .9Hz, ArH).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,33252-64-1, 3-Nitro-5-(trifluoromethyl)pyridin-2(1H)-one, and friends who are interested can also refer to it.

Reference:
Patent; NOVARTIS AG; LEGRAND, Darren Mark; WO2013/38373; (2013); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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. 33252-64-1, name is 3-Nitro-5-(trifluoromethyl)pyridin-2(1H)-one, molecular formula is C6H3F3N2O3, 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. Recommanded Product: 33252-64-1

(2) 52g of compound 2 was added to 150ml of phosphorus oxychloride,With stirring slowly add 21g of quinoline,Control feeding speed,So that the internal temperature does not exceed 50 degrees,At the same time compound 2 slowly dissolved,Argon gas protection system, oil bath heating,Set the external temperature 120 degrees,20-30 minutes after the system began to reflow,Maintain the system slightly boiled for 1.5 hours.TLC showed the reaction of raw materials is completed, stop heating,The system was concentrated under reduced pressure to remove phosphorus oxychloride, then dissolved in EA (400 ml) and the quinoline was removed by washing with 2N HCl (200 ml * 2)The mixture was washed with saturated sodium bicarbonate solution to neutrality and the organic phase was dried to give compound 3.TLC information: Raw material Rf = 0.1,Product Rf = 0.7. Developing agent: PE / EA / = 15/1.Measured product 50 grams, brown oil, yield 88%

With the rapid development of chemical substances, we look forward to future research findings about 33252-64-1.

Reference:
Patent; Si Fenke Si Pharmaceutical Research And Development (Tianjin) Co., Ltd.; Yao Qingjia; Li Changyong; Xu Yangjun; (8 pag.)CN105111209; (2017); B;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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. 33252-64-1, name is 3-Nitro-5-(trifluoromethyl)pyridin-2(1H)-one. This compound has unique chemical properties. The synthetic route is as follows. Quality Control of 3-Nitro-5-(trifluoromethyl)pyridin-2(1H)-one

To a solution of phosphoryl chloride (2.0 mL, 21.2 mmol) and quinoline (1.30 mL, 10.8 mmol) was added solid powder 3-nitro-5-(trifluoromethyl)pyridin-2-ol (4.00 g, 18.3 mmol) (95% purity). The resulting dark brown thick suspension was heated to reflux for 4 h and gradually turned into a very cloudy dark brown solution. After cooling to 100 C., water (11 mL) was slowly added to the mixture which was further cooled to room temperature and neutralized carefully with Na2CO3. The resulting solution was extracted with EtOAc three times. The extracts were combined, dried over MgSO4, filtered, and evaporated in vacuo. The residue was purified by flash chromatography on silica gel (EtOAc/hexanes 30:70) to afford 2.28 g of desired product.

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, 33252-64-1, 3-Nitro-5-(trifluoromethyl)pyridin-2(1H)-one.

Reference:
Patent; Xue, Chu-Biao; Zheng, Changsheng; Feng, Hao; Xia, Michael; Glenn, Joseph; Cao, Ganfeng.; Metcalf, Brian W.; US2006/4018; (2006); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem