HRID1059439
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 0.259 g of (10H-pyrazino[2,3-b][1,4]benzothiazin-8-yl)acetic acid in tetrahydrofuran (10 ml) was added in a nitrogen atmosphere 0.18 g of carbonyldiimidazole and the resulting mixture was heated under reflux for 30 minutes. Then the reaction mixture was brought back to room temperature and 0.285 g of methanesulfonamide was added thereto. After stirring at room temperature for 16 hours, the solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol) to thereby give 0.163 g of the title compound as a yellow solid.
WORKUP
后处理
- temperaturethe resulting mixture was heated
- temperatureunder reflux for 30 minutes
- customwas brought back to room temperature
- distillationthe solvent was distilled off under reduced pressure
- customthe residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol)