反应详情

Into a solution of 7 g of 10H-pyrazino[2,3-b][1,4]benzothiazine-8-methanol and 6.1 ml of pyridine in N,N-dimethylformamide (50 ml) was added dropwise 5.9 ml of methanesulfonyl chloride at 0° C. After stirring at room temperature for 1 hour, the reaction mixture was poured into a pre-cooled aqueous solution of methylene chloride/sodium hydrogencarbonate, extracted with ethyl acetate, washed with water and dried over anhydrous sodium sulfate. After distilling off the solvent under reduced pressure, the crystals thus precipitated were diluted with a small amount of ethyl acetate, taken up by filtration and washed with diethyl ether. Thus 4.7 g of the title compound was obtained as a yellow powder.

1. extractionextracted with ethyl acetate
2. washwashed with water
3. dry with materialdried over anhydrous sodium sulfate
4. distillationAfter distilling off the solvent under reduced pressure
5. customthe crystals thus precipitated
6. additionwere diluted with a small amount of ethyl acetate
7. filtrationtaken up by filtration
8. washwashed with diethyl ether