反应详情

温度

80 °C

A mixture of compound (500 mg) from Step 1 and P4S10(2.0 g) in 20 mL of pyridine is heated at 80° C. with stirring overnight. It is cooled and evaporated under vacuum, then diluted with water and stirred. The insoluble material is filtered and the mother liquid is extracted with CH2Cl2/EtOAc (1:4). The combined extract is washed with brine, dried and concentrated to give 120 mg of 4-thioxo-1,4,5,6,7,8-hexahydro-pyrrolo[3,2-c]azepine-3-carboxylic acid propyl ester.

1. temperatureIt is cooled
2. customevaporated under vacuum
3. additiondiluted with water
4. stirringstirred
5. filtrationThe insoluble material is filtered
6. extractionthe mother liquid is extracted with CH2Cl2/EtOAc (1:4)
7. extractionThe combined extract
8. washis washed with brine
9. customdried
10. concentrationconcentrated