HRID1582106

反应详情

EQUATION

反应方程式

HRID 1582106 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 1.90 g (7.13 mmol) [2-methoxy-5-(tetrahydro-pyran-4-yl)-phenyl]-thiourea in 50 ml chloroform was added dropwise 0.37 ml (7.22 mmol) bromine and the mixture heated at reflux for 18 hours. The mixture was then concentrated in vacuo. The residue was recrystallised from ethyl acetate to afford 920 mg (49%) 4-methoxy-7-(tetrahydro-pyran-4-yl)-benzothiazol-2-ylamine as a white solid. ES-MS m/e (%): 265 (M+H+, 100).

WORKUP

后处理

  1. temperaturethe mixture heated
  2. temperatureat reflux for 18 hours
  3. concentrationThe mixture was then concentrated in vacuo
  4. customThe residue was recrystallised from ethyl acetate