HRID493458

反应详情

EQUATION

反应方程式

HRID 493458 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a cooled (0° C.) solution of allyltrichlorosilane (4.9 mL; 34 mmol) in CH2Cl2 (50 mL) was added 1,8-Diazabicyclo[5.4.0]undec-7-ene (13 mL; 84 mmol). A solution of pinacol (4.0 g; 34 mmol) in CH2Cl2 (50 mL) was then added slowly and the resultant solution was warmed to room temperature and stirred for 12 hours. The solution was concentrated and the residue was treated with diethylether (100 mL). The mixture was stirred for 1 hour during which time the formation of a precipitate was observed. The mixture was then filtered and the filtrate was concentrated. The residue was distilled under reduced pressure to give 5.2 g (72%) of 2-allyl-2-chloro-4,4,5,5-tetramethyl-[1,3,2]dioxasilolane as a clear, colorless liquid.

WORKUP

后处理

  1. concentrationThe solution was concentrated
  2. additionthe residue was treated with diethylether (100 mL)
  3. stirringThe mixture was stirred for 1 hour during which time the formation of a precipitate
  4. filtrationThe mixture was then filtered
  5. concentrationthe filtrate was concentrated
  6. distillationThe residue was distilled under reduced pressure