HRID1866547

反应详情

EQUATION

反应方程式

HRID 1866547 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A mixture of 3-(2-[(2R)-2-(tert-butyldimethylsilanyloxy)-2-(4-hydroxy-3-hydroxymethyl-phenyl)ethylamino]-2-methylpropyl}benzoic acid methyl ester (preparation 36), (4.0 g, 8.21 mmol) and ammonium fluoride (3.04 g, 82.0 mmol) in methanol (20 mL) and water (5 mL) was heated at 40° C. for 18 hours. The reaction mixture was then concentrated in vacuo and the residue was purified by column chromatography on silica gel, eluting with dichloromethane:methanol: 0.88 ammonia, 100:0:0 to 90:10:0.1, to afford the title compound as a white foam in 81% yield, 2.42 g.

WORKUP

后处理

  1. concentrationThe reaction mixture was then concentrated in vacuo
  2. customthe residue was purified by column chromatography on silica gel
  3. washeluting with dichloromethane