HRID1288259

反应详情

EQUATION

反应方程式

HRID 1288259 的结构方程式

PROCEDURE

实验过程

Dimethylamino tributyltin (33.4 g.; 0.1 moles) and dimethylsulfoxide (100 g.; 1.28 moles) were stirred in a 250 ml reaction flask, under a positive pressure argon atmosphere, for 4.5 hours at 80° C. During the reaction, liberated dimethylamine gas exited from the reaction flask through an open port with the moving argon gas. The reaction stood overnight at ambient temperature. Excess dimethylsulfoxide was distilled at 75° C at 15 mm Hg. The reaction product was distilled through a semi-micro distillation apparatus at 138° C at 0.1 mm Hg. Yield of 25 g (68%) was identified as (methylsulfinylmethyl) tributyltin by 'H NMR and infrared spectra.

WORKUP

后处理

  1. customDuring the reaction
  2. distillationExcess dimethylsulfoxide was distilled at 75° C at 15 mm Hg
  3. distillationThe reaction product was distilled through a semi-micro distillation apparatus at 138° C at 0.1 mm Hg