HRID1013147

反应详情

EQUATION

反应方程式

HRID 1013147 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

To a mixture of 2-(2-iodo-benzyl)-isothiourea (13.53 g, 36.2 mmol) from previous step and a solution of NaOH (22 mL) in water (15 mL) was added dropwise dimethylsulfate (4.1 mL, 43.4 mmol). The reaction mixture was heated to reflux (105° C.) for 2 h, cooled. The resulting oil was then extracted into diethyl oxyde, the organic layer was washed with water, dried over Na2SO4. On concentration the solution generated a yellow oil that was directly used in the next step without any further purification (8.5 g, yield=89%).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperaturecooled
  3. extractionThe resulting oil was then extracted into diethyl oxyde
  4. washthe organic layer was washed with water
  5. dry with materialdried over Na2SO4
  6. concentrationOn concentration the solution
  7. customwas directly used in the next step without any further purification (8.5 g, yield=89%)