HRID2039442

反应详情

EQUATION

反应方程式

HRID 2039442 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of the above 1-[2-(3,5-dimethylphenyl)-1-(5,6,7,8-tetrahydronaphthalen-1-yl)-ethyl]-3-(2-hydroxyethyl)-thiourea (1.21 g) and concentrated hydrochloric acid (20 ml) was heated under reflux for 2 hours. The hydrochloric acid phase was decanted carefully and the remainder dissolved in ethyl acetate and washed three times with potassium carbonate solution (5 wt % in water), three times with water and dried over sodium sulphate. The solvent was removed by evaporation and the remainder triturated with a solution of light petrol ether/ethyl acetate (10/1) and the precipitate separated by filtration to yield the product C.2 as an off-white solid (1.02 g)

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. customThe hydrochloric acid phase was decanted carefully
  4. dissolutionthe remainder dissolved in ethyl acetate
  5. washwashed three times with potassium carbonate solution (5 wt % in water), three times with water
  6. dry with materialdried over sodium sulphate
  7. customThe solvent was removed by evaporation
  8. customthe remainder triturated with a solution of light petrol ether/ethyl acetate (10/1)
  9. customthe precipitate separated by filtration