HRID435061

反应详情

EQUATION

反应方程式

HRID 435061 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The alcohol of Example 3 (1 g) was dissolved in benzene (15 ml) and phenylisocyanate (600 mg) and a few drops of triethylamine were added. The mixture was refluxed for 20 hours. The solvent was then evaporated and the residue was taken up in ethyl acetate, washed with dilute hydrochloric acid and then with brine, dried over magnesium sulphate and evaporated down. The residue was purified on a silica column using 5% acetone in petrol as eluant. 1.4 g, corresponding to a 100% yield, of the desired product, as a viscous oil, were obtained. NMR showed the presence of both geometric isomers.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 20 hours
  2. customThe solvent was then evaporated
  3. washwashed with dilute hydrochloric acid
  4. dry with materialwith brine, dried over magnesium sulphate
  5. customevaporated down
  6. customThe residue was purified on a silica column