HRID916056

反应详情

EQUATION

反应方程式

HRID 916056 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A solution of 2-(3-{(2R)-2-[(2R)-2-{[tert-butyl(dimethyl)silyl]oxy}-2-(4-hydroxy-3-hydroxymethyl-phenyl)-ethylamino]-propyl}-phenyl)-N-(2,6-dimethoxybenzyl)-acetamide (Preparation 1) (125 mg, 0.20 mmol) in methanol (6 ml) was treated with acetic acid (6 ml) and ammonium fluoride (74 mg, 2.0 mmol) and the reaction heated to 40° C. for 16 hours. The solvent was removed in vacuo and the residue purified by flash column chromatography on silica gel eluting with dichloromethane:methanol:880 ammonia (95:5:0.5 changing to 93:7:0.7, by volume) to give the title compound as a white solid after trituration with diethyl ether (59 mg).

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. customthe residue purified by flash column chromatography on silica gel eluting with dichloromethane