HRID924725

反应详情

EQUATION

反应方程式

HRID 924725 的结构方程式

PROCEDURE

实验过程

A solution of 2-(4-bromophenyl)-oxirane (0.5 g, 2.51 mmol) in methylamine (6.6 ml, 33% by volume in ethanol, 25.12 mmol) was stirred at room temperature under an atmosphere of nitrogen. After 18 hours the solvent was removed in vacuo and the residue was purified over flash silica eluting with dichloromethane: methanol:acetic acid:water (120:15:3:2) to afford the desired compound as the acetic acid salt. Further purification over a Phenomenex_Strata_SCX column eluting with methanol followed by 2N ammonia in methanol gave the desired product. LC/MS: (PS-B3) Rt 2.52 [M+H]+ 230.

WORKUP

后处理

  1. customAfter 18 hours the solvent was removed in vacuo
  2. customthe residue was purified over flash silica eluting with dichloromethane: methanol:acetic acid:water (120:15:3:2)