반응 #42889

반응 방정식

triethylamine

4-amino-thiophene-3-carboxylic acid methyl ester

2-chloropropionyl chloride

→

title compound

수율 82.0%

rac-4-(2-Chloro-propionylamino)-thiophene-3-carboxylic acid methyl ester

수율 82.0%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   온도to warm up to room temperature
2. 2
   세척the solution was washed twice with water
3. 3
   건조dried over sodium sulfate
4. 4
   농축concentrated in vacuo
5. 5
   기타The residue was purified by column chromatography

실험 절차

To a suspension of 4-amino-thiophene-3-carboxylic acid methyl ester (2.0g) in dichloromethane (25 mL) was added 2-chloropropionyl chloride (1.13 mL). The reaction mixture was then cooled down to −15° C. and a solution of triethylamine (3.2 mL) in dichloromethane (5 mL) was slowly added over 30 minutes. After such time the reaction mixture was allowed to warm up to room temperature, and the solution was washed twice with water, dried over sodium sulfate and then concentrated in vacuo. The residue was purified by column chromatography to yield the title compound as a light yellow solid (2.1g, 82%). MS (EI): 247.0.

출처