HRID1248932

反应详情

EQUATION

反应方程式

HRID 1248932 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

A solution of benzylamine (5.4 g, 0.05 mole) and triethylamine (15.4 ml, 0.11 mole) in 50 ml of tetrahydrofuran was added dropwise to a solution of thiophosgene (4.2 ml, 0.055 mole) in 50 ml of tetrahydrofuran with cooling to -10° C. over a period of twenty minutes. The mixture was stirred at 25° C. for 2.75 hours and filtered. The filtrate was treated with charcoal, then filtered and evaporated to an oil. The oil was diluted with hexane:ethyl acetate (90:10) and purified on a flash silica column using hexane:ethyl acetate (90:10) as the eluant to yield benzyl isothiocyanate as a yellow oil.

WORKUP

后处理

  1. filtrationfiltered
  2. additionThe filtrate was treated with charcoal
  3. filtrationfiltered
  4. customevaporated to an oil
  5. additionThe oil was diluted with hexane:ethyl acetate (90:10)
  6. custompurified on a flash silica column