HRID1772569

反应详情

EQUATION

反应方程式

HRID 1772569 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Tetrahydrofuran (82 mL) and n-decyltrichlorosilane (Tokyo Chemical Industry Co., Ltd., 14.5 g, 52.6 mmol) were placed in a 500 mL four-necked flask in a nitrogen atmosphere, and cooled to 0° C. n-decyl magnesium bromide (Sigma-Aldrich Co. LLC., 1.0 M, 58 ml) was added dropwise, and the mixture was agitated for 1 hour at 10° C. or less. The temperature was raised gradually to room temperature over the course of about 1 hour, and the mixture was left standing overnight. The precipitated salt was filtered out, the tetrahydrofuran was removed by concentration under reduced pressure, and distillation under reduced pressure was performed to obtain the target dichlorodi-n-decylsilane (Compound E21) (150° C./0.1-0.2 Torr, 13.1 g, yield 65%).

WORKUP

后处理

  1. additionwas added dropwise
  2. waitthe mixture was left
  3. waitstanding overnight
  4. filtrationThe precipitated salt was filtered out
  5. customthe tetrahydrofuran was removed by concentration under reduced pressure, and distillation under reduced pressure