反应详情

A stirred mixture of 2-amino-4-chloromethylthiazole hydrochloride (0.7 g), 4-(diphenylmethoxy)piperidine (0.78 g) and triethylamine (1.82 ml) in N,N-dimethylformamide (7.8 ml) was heated at 40° C. to 45° C. for 5 hours. After cooling to ambient temperature, the reaction mixture was filtered. The filtrate was poured into water (50 ml) and extracted with ethyl acetate (80 ml×2). The extract was washed with a saturated aqueous solution of sodium chloride (30 ml) and dried over magnesium sulfate. The solvent was distilled off and the residue was subjected to column chromatography on silica gel (30 g) 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 to give 2-amino-4-[4-(diphenylmethoxy)piperidinomethyl]thiazole (0.78 g).

1. temperaturewas heated at 40° C. to 45° C. for 5 hours
2. filtrationthe reaction mixture was filtered
3. additionThe filtrate was poured into water (50 ml)
4. extractionextracted with ethyl acetate (80 ml×2)
5. washThe extract was washed with a saturated aqueous solution of sodium chloride (30 ml)
6. dry with materialdried over magnesium sulfate
7. distillationThe solvent was distilled off
8. washeluted with a mixture of chloroform and methanol (10:1 V/V)
9. additionThe fractions containing the object compound
10. concentrationconcentrated under reduced pressure