反应详情

A stirred mixture of 4-chloromethyl-2-propionylaminothiazole (0.64 g), 4-(diphenylmethoxy)piperidine (0.8 g) and sodium bicarbonate (0.3 g) in N,N-dimethylformamide (8 ml) was heated at 80° to 90° C. for 2 hours. The reaction mixture was poured into ice water. The resulting precipitate was collected, washed with water and dried in vacuo. The precipitate was subjected to column chromatography on silica gel and eluted with a mixture of chloroform and methanol (10:1 V/V). The fractions containing the object compound were combined and concentrated under reduced pressure. The residue was triturated with diisopropyl ether to give white crystals. The crystals were recrystallized from a mixture of toluene and diisopropyl ether and dried under reduced pressure to give 2-propionylamino-4-[4-(diphenylmethoxy)piperidinomethyl]thiazole (0.35 g).

1. temperaturewas heated at 80° to 90° C. for 2 hours
2. customThe resulting precipitate was collected
3. washwashed with water
4. customdried in vacuo
5. washeluted with a mixture of chloroform and methanol (10:1 V/V)
6. additionThe fractions containing the object compound
7. concentrationconcentrated under reduced pressure
8. customThe residue was triturated with diisopropyl ether
9. customto give white crystals
10. customThe crystals were recrystallized from a mixture of toluene and diisopropyl ether
11. customdried under reduced pressure