HRID9702

反应详情

EQUATION

反应方程式

HRID 9702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

340 g (6.3 mol) of sodium methylate (95% strength) are dissolved in portions in 2.5 l of methanol in a laboratory reactor blanketed with nitrogen. During this procedure, the solution heats up to 65° C. Thereafter, 995 g (5.8 mol) of chloromethyltrimethoxysilane are added dropwise over 1.5 h and stirring is effected for a further 30 minutes at the boil. On addition of the silane, sodium chloride is precipitated spontaneously as the salt, but the suspension remains readily stirrable until the end of the metering. The precipitated sodium chloride is filtered off with suction and the methanol is removed under a partial vacuum at 40–50° C. The residue is purified by distillation (97–98° C. at 172 mbar).

WORKUP

后处理

  1. customheats up to 65° C
  2. customis precipitated spontaneously as the salt
  3. filtrationThe precipitated sodium chloride is filtered off with suction
  4. customthe methanol is removed under a partial vacuum at 40–50° C
  5. distillationThe residue is purified by distillation (97–98° C. at 172 mbar)