反应详情

3.06 g of 3,4-diaminothiophene were mixed with 45 ml of methylene chloride and 9 ml of triethylamine and a solution of 3.6 g of valeroyl chloride in 45 ml of methylene chloride was added at a temperature of 20° C. over one hour. The mixture was stirred for 30 minutes, followed by evaporation to dryness. After separation by chromatography (eluant: methanol/methylene chloride 5/95), 3.2 g of the expected monoamide were obtained which was crystallized from 15 ml of a 50/50 mixture of isopropyl ether and cyclohexane. The crystals were separated, washed with this mixture and dried under reduced pressure at 100° C. to obtain 2.14 g of the expected product melting at 110° C.

1. customfollowed by evaporation to dryness
2. customAfter separation by chromatography (eluant: methanol/methylene chloride 5/95), 3.2 g of the expected monoamide
3. customwere obtained which
4. customwas crystallized from 15 ml of a 50/50 mixture of isopropyl ether and cyclohexane
5. customThe crystals were separated
6. washwashed with this mixture
7. customdried under reduced pressure at 100° C.