Category: 251101-36-7

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.251101-36-7, name is 3-Methylisonicotinamide, molecular formula is C7H8N2O, molecular weight is 136.15, as common compound, the synthetic route is as follows.HPLC of Formula: C7H8N2O

3-Methyl-4-cyanopyridine (123) Phosphorus oxychloride (100 mL, 1.1 mol) was slowly added to the crude amide 122 (15 g, 0.11 mol) while cooling the mixture in an ice bath. The resulting solution was heated at reflux for 24 h. The reaction mixture was cooled to room temperature and the excess phosphorus oxychloride was removed under reduced pressure. Crushed ice (150 g) was slowly added to the oily residue, and the solution was neutralized with saturated ammonium hydroxide. The crude product was extracted with chloroform (3*100 mL). The combined extracts were filtered through a layer of silica gel, washing with extra portions of chloroform. The filtrates were evaporated to dryness to yield 123 as colorless crystals (12 g, 90%): mp 45-47 C. (lit. (J. Med. Chem. 2000, 43, 3168-3185) mp 50 C.). 1H NMR (300 MHz, CDCl3) delta 8.66 (s, 1H), 8.59 (d, J=5.0 Hz, 1H), 7.45 (d, J=5.0 Hz, 1H), 2.54 (s, 3H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,251101-36-7, 3-Methylisonicotinamide, and friends who are interested can also refer to it.

Reference:
Patent; CUSHMAN, Mark S.; KISELEV, Evgeny A.; MORRELL, Andrew E.; US2014/18360; (2014); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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. 251101-36-7, name is 3-Methylisonicotinamide, the common compound, a new synthetic route is introduced below. SDS of cas: 251101-36-7

Phosphorus oxychloride (2 mL) was slowly added to a stirred 3-Methylisonicotinamide (25, 300 mg, 2.2 mmol). The resulting solutionwas heated to reflux for 24 h, then reaction mixture was cooled to roomtemperature, and the excess phosphorus oxychloride was removedunder reduced pressure. Crushed ice was slowly added to the oily residue,and the solution was neutralized with saturated aqueous sodiumcarbonate solution. The crude product was extracted with EtOAc(3×25 mL), and combined organic extracts were washed with brine,dried over anhydrous sodium sulfate, filtered, and concentrated underreduced pressure. Resulting residue was purified by flash columnchromatography on silica gel (EtOAc/Petroleum ether 1:4) to yield thewhite solid (65%). 1H NMR (400 MHz, CDCl3) delta 8.67 (s, 1H), 8.59 (d,J=5.0 Hz, 1H), 7.46 (d, J=5.0 Hz, 1H), 2.54 (s, 3H).

The synthetic route of 251101-36-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Qin, Li-Huai; Wang, Zhi-Long; Xie, Xin; Long, Ya-Qiu; Bioorganic and Medicinal Chemistry; vol. 26; 12; (2018); p. 3559 – 3572;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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. 251101-36-7, name is 3-Methylisonicotinamide, the common compound, a new synthetic route is introduced below. SDS of cas: 251101-36-7

Phosphorus oxychloride (2 mL) was slowly added to a stirred 3-Methylisonicotinamide (25, 300 mg, 2.2 mmol). The resulting solutionwas heated to reflux for 24 h, then reaction mixture was cooled to roomtemperature, and the excess phosphorus oxychloride was removedunder reduced pressure. Crushed ice was slowly added to the oily residue,and the solution was neutralized with saturated aqueous sodiumcarbonate solution. The crude product was extracted with EtOAc(3×25 mL), and combined organic extracts were washed with brine,dried over anhydrous sodium sulfate, filtered, and concentrated underreduced pressure. Resulting residue was purified by flash columnchromatography on silica gel (EtOAc/Petroleum ether 1:4) to yield thewhite solid (65%). 1H NMR (400 MHz, CDCl3) delta 8.67 (s, 1H), 8.59 (d,J=5.0 Hz, 1H), 7.46 (d, J=5.0 Hz, 1H), 2.54 (s, 3H).

The synthetic route of 251101-36-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Qin, Li-Huai; Wang, Zhi-Long; Xie, Xin; Long, Ya-Qiu; Bioorganic and Medicinal Chemistry; vol. 26; 12; (2018); p. 3559 – 3572;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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. 251101-36-7, name is 3-Methylisonicotinamide, the common compound, a new synthetic route is introduced below. SDS of cas: 251101-36-7

Phosphorus oxychloride (2 mL) was slowly added to a stirred 3-Methylisonicotinamide (25, 300 mg, 2.2 mmol). The resulting solutionwas heated to reflux for 24 h, then reaction mixture was cooled to roomtemperature, and the excess phosphorus oxychloride was removedunder reduced pressure. Crushed ice was slowly added to the oily residue,and the solution was neutralized with saturated aqueous sodiumcarbonate solution. The crude product was extracted with EtOAc(3×25 mL), and combined organic extracts were washed with brine,dried over anhydrous sodium sulfate, filtered, and concentrated underreduced pressure. Resulting residue was purified by flash columnchromatography on silica gel (EtOAc/Petroleum ether 1:4) to yield thewhite solid (65%). 1H NMR (400 MHz, CDCl3) delta 8.67 (s, 1H), 8.59 (d,J=5.0 Hz, 1H), 7.46 (d, J=5.0 Hz, 1H), 2.54 (s, 3H).

The synthetic route of 251101-36-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Qin, Li-Huai; Wang, Zhi-Long; Xie, Xin; Long, Ya-Qiu; Bioorganic and Medicinal Chemistry; vol. 26; 12; (2018); p. 3559 – 3572;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem