반응 #2298629

ord-76c277f88a884fe49b4e2510066e5ae3

반응 방정식

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
수율 85.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

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 (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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE039267E1uspto-grants-2006_09