反应详情

温度

80 °C

To a solution of 100 mg of pyrazole in N,N-dimethylformamide was added in a nitrogen atmosphere 60 mg of sodium hydride (oily 60%) under ice cooling and the resulting mixture was stirred for 10 minutes. Subsequently, 240 mg of 10-methoxymethyl-8-chloromethyl-10H-pyrazino[2,3-b][1,4]benzothiazine was added to the reaction mixture, which was then heated to 80° C. for 10 minutes. Then the reaction mixture was brought back to room temperature and distributed into water and ethyl acetate. The organic layer was extracted, washed with water and dried over anhydrous sodium sulfate. After distilling off the solvent under reduced pressure, the residue thus obtained was purified by silica gel column chromatography (eluted with ethyl acetate/n-hexane) to thereby give 150 mg of the title compound as a yellow powder.

1. customwas brought back to room temperature
2. extractionThe organic layer was extracted
3. washwashed with water
4. dry with materialdried over anhydrous sodium sulfate
5. distillationAfter distilling off the solvent under reduced pressure
6. customthe residue thus obtained
7. customwas purified by silica gel column chromatography (eluted with ethyl acetate/n-hexane)