HRID911342

反应详情

EQUATION

反应方程式

HRID 911342 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Heat copper(I) cyanide (0.84 g, 9.4 mmol) and 6-bromobenzo[b]thiophene (prepared as described in WO 01/23381) (1.0 g, 4.7 mmol) at 160° C. for 13 h. Cool the mixture to 0° C., add 33% aqueous ethylenediamine (20 mL) and dilute with ether. Wash the organic mixture with brine, dry over Na2SO4 and evaporate. Purify by chromatography on silica gel eluting with EtOAc/hexane (0:1 to 1:3) to give the desired intermediate (0.58 g, 78%). GC-MS m/z: 159 (M+).

WORKUP

后处理

  1. washWash the organic mixture with brine
  2. dry with materialdry over Na2SO4
  3. customevaporate
  4. customPurify by chromatography on silica gel eluting with EtOAc/hexane (0:1 to 1:3)