HRID1776590
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of ethyl 4-methoxy-3-(N-(2-morpholinoethyl)-methylsulfonamido)-phenyl carbonate (0.250 g, 0.621 mmol) in MeOH (5 ml), LiOH 1M (1.242 ml, 1.242 mmol) was added, and the mixture was stirred at RT for 4 hours. The volatiles were removed under vacuum, and the solid residue was partitioned between EtOAc and a diluted aqueous solution of HCl (pH=5). The organic layer was dried over Na2SO4, the solvent was evaporated and the crude was purified by chromatography on silica gel column (DCM:MeOH=10:0.2) affording N-(5-hydroxy-2-methoxyphenyl)-N-(2-morpholinoethyl)methanesulfonamide (0.180 g, 0.545 mmol, 88% yield, MS/ESI+ 331.0 [MH]+).
WORKUP
后处理
- customThe volatiles were removed under vacuum
- customthe solid residue was partitioned between EtOAc
- dry with materialThe organic layer was dried over Na2SO4
- customthe solvent was evaporated
- customthe crude was purified by chromatography on silica gel column (DCM:MeOH=10:0.2)