反応 #2298618

ord-32c3794161204a7eb2dd3faa7b51ab85

反応方程式

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
収率 85.0%

反応条件

詳細条件
See reaction.notes.procedure_details.

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 (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.

出典

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