반응 #2298613

반응 방정식

acetic anhydride

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

→

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

수율 95.0%

용매

Formic acid

반응 조건

후처리

1. 1
   온도while cooling in an ice bath
2. 2
   기타The cooling bath was removed
3. 3
   workup.ADDITIONThe reaction mixture was diluted with water (100 mL)
4. 4
   여과the solid product collected by vacuum filtration

실험 절차

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.

출처