反应详情

A mixture of 2-propionylamino-4-chloromethylthiazol (5.11 g), 3-(4-piperidyl)indole (5 g), sodium hydrogen carbonate (2.31 g) and N,N-dimethylformamide (25 ml) was heated at 102° to 103° C. with bubbling nitrogen gas and stirring for 6 hours. The reaction mixture was filtered and the filtrate was concentrated. The residue was subjected to column chromatography on silica gel and the column was eluted with a mixture of chloroform and methanol (10:1 V/V). The fractions containing the desired compound were combined and concentrated and ethanol was added thereto. The solution was concentrated again and the residue was triturated with diisopropyl ether to give 4-[4-(3-indolyl)piperidinomethyl]-2-propionylaminothiazole (6.50 g).

1. temperaturewas heated at 102° to 103° C. with bubbling nitrogen gas
2. filtrationThe reaction mixture was filtered
3. concentrationthe filtrate was concentrated
4. washthe column was eluted with a mixture of chloroform and methanol (10:1 V/V)
5. additionThe fractions containing the desired compound
6. concentrationconcentrated
7. additionethanol was added
8. concentrationThe solution was concentrated again
9. customthe residue was triturated with diisopropyl ether