HRID1112186

反应详情

EQUATION

反应方程式

HRID 1112186 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Five milliliters of thionyl chloride are added to a solution of 5.0 g (30 millimoles) tricyclo [4.3.1.12,5 ] undecane-1-ol in 30 ml dry anhydrous benzene and the entirety is refluxed for 1.5 hours. The reaction mixture is concentrated under reduced pressure and there is further added 20 ml of dry benzene. Reduced pressure concentration is repeated to distill out the excess thionyl chloride completely. The residue is distilled under reduced pressure to collect a fraction boiling at 95° C./3mmHg, to obtain 5.0 g (yield 89%) of 1-chlorotricyclo [4.3.1.12,5 ] undecane.

WORKUP

后处理

  1. temperaturethe entirety is refluxed for 1.5 hours
  2. concentrationThe reaction mixture is concentrated under reduced pressure and there
  3. concentrationReduced pressure concentration
  4. distillationto distill out the excess thionyl chloride completely
  5. distillationThe residue is distilled under reduced pressure
  6. customto collect a fraction boiling at 95° C./3mmHg