HRID65558

反应详情

EQUATION

反应方程式

HRID 65558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N,N-Dibutylaminoethyl Tributylstannyl Ether is prepared from 59.6 gm (0.1 mole) bis(tributyltin) oxide and 34.6 gm (0.2 mole) N,N-dibutylethanolamine in 200 ml benzene. This is stirred and heated to reflux in a system that contains a Dean-Starke tube. After 30 minutes water began to collect in the Dean-Starke tube and after refluxing for a period of 22 hours a total of 1.8 ml of water (theory 1.8 ml) had collected. A rotating evaporator is used to remove the benzene and to provide 95.1 gm of red-orange liquid. This is fractionated at reduced pressure with collection at 163°-166° C. at 0.7 mm of 73.1 gm of yellow liquid (Percent yield - 79). Infrared spectral analysis shows this to be the desired ether.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux in a system that
  3. customto collect in the Dean-Starke tube
  4. temperatureafter refluxing for a period of 22 hours a total of 1.8 ml of water (theory 1.8 ml)
  5. customhad collected
  6. customA rotating evaporator
  7. customto remove the benzene