HRID2073917

反应详情

EQUATION

反应方程式

HRID 2073917 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Allyl glycidyl ether (57.1 g, 0.5 moles) was added to a 250 mL 3-neck flask, equipped with a stirrer, dropping funnel, internal thermometer and condenser, and heated to 100° C. After the addition of 1 mL of a 1 weight percent solution of hexachloroplatinic acid in diethylene glycol dimethyl ether, 24.0 g (0.1 moles) of 2,4,6,8-tetramethylcyclotetrasiloxane were added very rapidly with vigorous stirring, the internal temperature rising to 195° C. After the addition of 2,4,6,8-tetramethylcyclotetrasiloxane, stirring was continued until the temperature of the reaction product had dropped to 130° C. Unreacted portions of the allyl glycidyl ether and 2,4,6,8-tetramethylcyclotetrasiloxane were removed by stirring the reaction mixture at 60°-70° C. at a vacuum of 0.1 hPa, produced by an oil pump. The slightly yellowish crude product (77.8%), nD20 : 1.4633, was subjected to a fractional vacuum distillation using a packed column. The compound (21) distilled at about 335° C. and 1 hPa as a clear, viscous liquid, the greater portion polymerizing. nD20 : 1,4668.

WORKUP

后处理

  1. customequipped with a stirrer
  2. additionwere added very rapidly with vigorous stirring
  3. customrising to 195° C
  4. additionhad dropped to 130° C
  5. customwere removed
  6. stirringby stirring the reaction mixture at 60°-70° C. at a vacuum of 0.1 hPa
  7. customproduced by an oil pump
  8. distillationThe slightly yellowish crude product (77.8%), nD20 : 1.4633, was subjected to a fractional vacuum distillation
  9. distillationThe compound (21) distilled at about 335° C.
  10. custom1 hPa as a clear, viscous liquid, the greater portion polymerizing