反应详情

温度

70 °C

The mixture of ethyl (2E)-5-chloro-4-oxo-2-pentenoate (0.5 g) and N-[1-(4-chlorobenzoyl)-3-pyrrolidinyl]thiourea (0.8 g) in acetonitrile (10 mL) was stirred at 70° C. for 3 hours, and the mixture was evaporated in vacuo. To the residue was added a solution of AcOEt and water, and the mixture was adjusted to pH 8 with 20% aqueous potassium carbonate. The separated organic layer was washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by column chromatography on silica gel using AcOEt as an eluent. The eluted fractions containing the desired product were collected and evaporated in vacuo to give ethyl (2E)-3-(2-{[1-(4-chlorobenzoyl)-3-pyrrolidinyl]amino}-1,3-thiazol-4-yl)acrylate (1.0 g).

1. customthe mixture was evaporated in vacuo
2. additionTo the residue was added a solution of AcOEt and water
3. washThe separated organic layer was washed with water
4. dry with materialdried over magnesium sulfate
5. customevaporated in vacuo
6. customThe residue was purified by column chromatography on silica gel
7. additionThe eluted fractions containing the desired product
8. customwere collected
9. customevaporated in vacuo