HRID622711

反应详情

EQUATION

反应方程式

HRID 622711 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

A mixture of 9.3 g (0.04 mole) of 3-(2-guanidino-4-thiazolyl)benzeneamine, 20 ml of triethylorthoformate, and 2 drops of trifluoroacetic acid is stirred at reflux for 5 hours after which it is concentrated in vacuo. The residue is dissolved in 20 ml of ethanol, the solution cooled to 0° C. and then treated with excess sodium borohydride. The mixture is allowed to warm to room temperature, then stirred at reflux for 4 hours. Upon concentration in vacuo the residue is partitioned between water and dichloromethane.

WORKUP

后处理

  1. temperatureat reflux for 5 hours after which it
  2. concentrationis concentrated in vacuo
  3. dissolutionThe residue is dissolved in 20 ml of ethanol
  4. additiontreated with excess sodium borohydride
  5. temperatureto warm to room temperature
  6. stirringstirred
  7. temperatureat reflux for 4 hours
  8. concentrationUpon concentration in vacuo the residue
  9. customis partitioned between water and dichloromethane