反应 #2298618

ord-32c3794161204a7eb2dd3faa7b51ab85

反应方程式

CC(=O)OC(C)=O
acetic anhydride
COC(=O)c1sccc1N
3-amino-2-thiophenecarboxylic acid methyl ester
COC(=O)c1sccc1NC=O
3-(formylamino)-2-thiophenecarboxylic acid methyl ester
收率 85.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

Formic acid (40 mL) was added to acetic anhydride (60 mL) while cooling in an ice bath. Solid 3-amino-2-thiophenecarboxylic acid methyl ester (77, 10.3 g, 66 mmol) 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)-2-thiophenecarboxylic acid methyl ester (10.3 g, 85% yield) as a white solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE039267E1uspto-grants-2006_09