HRID1681344

反应详情

EQUATION

反应方程式

HRID 1681344 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of trans-stilbene oxide (1.96 g, 0.010 mol) and tetrahydrofurfurylamine (3.03 g, 0.030 mol) was heated at 140° C. for 2 hours. After standing at ambient temperature for 18 hours the mixture was diluted with water (150 mL). An oil separated from the solution but solidified on standing for an hour. NMR and mass spectral analyses showed stilbene oxide remaining. The solid was treated with another 3.03 g of tetrahydrofurfurylamine and the mixture heated at 150° C. for another 3 hours. The reaction mixture was treated with water (150 mL) as before to obtain 2.28 g (77%) of an off-white solid after drying under ambient conditions for 18 hours. The solid was recrystallized form toluene; mp 167°-168° C.

WORKUP

后处理

  1. customAn oil separated from the solution
  2. waiton standing for an hour
  3. additionThe solid was treated with another 3.03 g of tetrahydrofurfurylamine
  4. temperaturethe mixture heated at 150° C. for another 3 hours
  5. additionThe reaction mixture was treated with water (150 mL) as before