反応 #2298613

反応方程式

acetic anhydride

methyl 3-amino-4-methyl-2-thiophenecarboxylic acid methyl ester

→

3-(formylamino)-4-methyl-2-thiophenecarboxylic acid methyl ester

収率 95.0%

溶媒

Formic acid

反応条件

後処理

1. 1
   温度while cooling in an ice bath
2. 2
   その他The cooling bath was removed
3. 3
   workup.ADDITIONThe reaction mixture was diluted with water (100 mL)
4. 4
   ろ過the solid product collected by vacuum filtration

実験手順

Formic acid (53 mL) was added to acetic anhydride (53 mL) while cooling in an ice bath. Solid methyl 3-amino-4-methyl-2-thiophenecarboxylic acid methyl ester (1, 18.2 g, 0.11 mol) was added to the cold solution in small portions. The cooling bath was removed and the resulting suspension was stirred at room temperature for 4 hours. The reaction mixture was diluted with water (100 mL) and the solid product collected by vacuum filtration to yield 3-(formylamino)-4-methyl-2-thiophenecarboxylic acid methyl ester (20.2 g, 95% yield) as a white solid.

出典