Ammonia → 2-Chloro-4-methylpyridine-3-carboxamide
反応式
[Cl:1][C:2]1[C:7]([C:8](O)=[O:9])=[C:6]([CH3:11])[CH:5]=[CH:4][N:3]=1.O=S(Cl)Cl.[NH3:16]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[C:7]([C:8]([NH2:16])=[O:9])=[C:6]([CH3:11])[CH:5]=[CH:4][N:3]=1参加物
5
実験手順
To a mixture of 2-chloro-4-methyl-3-pyridinecarboxylic acid (24.7 g, 157 mmol) and 75 mL of toluene at 70° C. was added 75 mL of SOCl2 (22.6 g, 190 mmol) within a period of 1 hour. The reaction mixture was refluxed for 4 hours and the resulting solution was cooled to room temperature. Dry NH3 gas was introduced at such a rate so as to maintain the internal temperature below 30° C. After removing toluene, the solid residue was washed successively with cold water and methanol, and dried to yield 22.72 g of the title compound (91%, m.p. 168°-170° C.).
後処理
- temperatureThe reaction mixture was refluxed for 4 hours
- temperatureto maintain the internal temperature below 30° C
- customAfter removing toluene
- washthe solid residue was washed successively with cold water and methanol
- customdried
出典と根拠
- ORDレコード
- ord-7153c737860b4ca2803911bb6ce5a8eb
- 出典データセット
- uspto-grants-1996_02
- 特許番号
- US05493028
反応ノート
読み込み中…