HRID352771
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 1-tert-butoxycarbonyl-4-[(5-chloro-1-phenylsulfonylindol-2-yl)sulfonyl]piperazine (4.84 g), a 0.5N methanol solution of sodium hydroxide (20 ml) was added, followed by stirring at room temperature for 1 hour. Under ice cooling, a saturated aqueous solution of ammonium chloride was added to the reaction mixture. Water and dichloromethane were then added to separate the organic layer. The organic layer was dried over anhydrous sodium sulfate. The residue obtained by distilling off the solvent under reduced pressure was purified by chromatography on a silica gel column (methanol:dichloromethane=1:20), whereby the title compound (3.33 g, 93%) was obtained as colorless powder.
WORKUP
后处理
- customto separate the organic layer
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- customThe residue obtained
- distillationby distilling off the solvent under reduced pressure
- customwas purified by chromatography on a silica gel column (methanol:dichloromethane=1:20), whereby the title compound (3.33 g, 93%)
- customwas obtained as colorless powder