تفاعل #42889

معادلة التفاعل

triethylamine

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

2-chloropropionyl chloride

→

title compound

المردود 82.0%

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

المردود 82.0%

المذيبات

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto warm up to room temperature
2. 2
   غسيلthe solution was washed twice with water
3. 3
   تجفيفdried over sodium sulfate
4. 4
   تركيزconcentrated in vacuo
5. 5
   أخرىThe residue was purified by column chromatography

الإجراء التجريبي

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.

المصدر