HRID1776590

反应详情

EQUATION

反应方程式

HRID 1776590 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe volatiles were removed under vacuum
  2. customthe solid residue was partitioned between EtOAc
  3. dry with materialThe organic layer was dried over Na2SO4
  4. customthe solvent was evaporated
  5. customthe crude was purified by chromatography on silica gel column (DCM:MeOH=10:0.2)