HRID395272

反应详情

EQUATION

反应方程式

HRID 395272 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-(tert-butyloxycarbonyl)-7-hydroxy-2,3,4,5-tetrahydro-1H-3-benzazepine (3.0 g, 0.011 mol), methanesulphonylchloride (1.44 g, 0.013 mol), triethylamine (1.27 g, 0.013 mol) and dichloromethane (50 ml) was stirred at room temperature for 18 h. The reaction mixture was then partitioned between dichloromethane (50 ml) and a saturated solution of sodium hydrogen carbonate (50 ml). The organic layer was separated, washed with water (50 ml) and then dried (Na2SO4). The solvent was then evaporated in vacuo to give the title compound (3.85 g, 99%) as a pale yellow oil.

WORKUP

后处理

  1. customThe reaction mixture was then partitioned between dichloromethane (50 ml)
  2. customThe organic layer was separated
  3. washwashed with water (50 ml)
  4. dry with materialdried (Na2SO4)
  5. customThe solvent was then evaporated in vacuo