反应详情

1.25 g of 8-aminomethyl-10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine and 0.7 ml of triethylamine were dissolved in N,N-dimethylformamide (15 ml). Under ice-cooling, 2 ml of a solution of 0.4 ml of chloroacetyl chloride in dichloromethane was dropped thereinto and the resulting mixture was stirred for 1 hour. After adding water, the reaction mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water and a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. After concentrating under reduced pressure, the residue was purified by silica gel column chromatography (eluted with n-hexane/ethyl acetate). The crystals thus obtained were washed with n-hexane and thus 1.28 g of the title compound was obtained as a yellow powder.

1. temperatureUnder ice-cooling
2. extractionthe reaction mixture was extracted with ethyl acetate
3. washThe ethyl acetate layer was washed with water
4. dry with materiala saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate
5. concentrationAfter concentrating under reduced pressure
6. customthe residue was purified by silica gel column chromatography (eluted with n-hexane/ethyl acetate)
7. customThe crystals thus obtained
8. washwere washed with n-hexane