3-Methylpicolinamide synthesis
- Product Name:3-Methylpicolinamide
- CAS Number:937648-82-3
- Molecular formula:C7H8N2O
- Molecular Weight:136.15
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Yield:937648-82-3 97%
Reaction Conditions:
with sulfuric acid at 20 - 80; for 0.416667 h;
Steps:
8 Example 8rac-N-(((2S,3R)-3 -Methyl-i -(2-methyl-S -phenylthiazole-4-carbonyl)piperidin-2- ylmethyliuinoline-8-carboxamide
Example 8rac-N-(((2S,3R)-3 -Methyl-i -(2-methyl-S -phenylthiazole-4-carbonyl)piperidin-2- ylmethyliuinoline-8-carboxamide3 -MethylpicolinamideLN_I,NH20A mixture of 3-methylpicolinonitrile (2.36 g, 20 mmol) and conc. sulfuric acid (12.5mL) was stirred at 80°C for 25 mm. The solution was cooled to r.t., poured into water (80mL), followed by addition of sat. Na2CO3 (aq.) until pH 7. The resulting mixture was extracted with DCM (3x) and the combined organic layer was dried over Mg504 and concentrated in vacuo to provide 3-methylpicolinamide as a white solid (2.65 g, 97%). ‘H74NMR (CDC13, 400 MHz) ? 8.43 (dd, 1H), 7.93 (brs, 1H), 7.62 (dd, 1H), 7.35 (dd, 1H), 5.44 (brs, 1H), 2.76 (s, 3H).
References:
WO2013/119639,2013,A1 Location in patent:Page/Page column 74; 75
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