反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Six milliliters (78 millimoles) of thionyl bromide are added to 20 ml of a solution of 5.36 g (32 millimoles) of tricyclo [4.3.1.12,5 ] undecane-1-ol in dry 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 96°-8° C./2mmHg. Thus 4.53 g (yield 61.3%) of 1-bromotricyclo [4.3.1.12,5 ] undecane are obtained. After cooling, colorless crystals having a melting point of 57.7°-58.5° C. are obtained. The properties of this product are the same as those shown in Example 1.
WORKUP
后处理
- temperaturethe entirety is refluxed for 1.5 hours
- concentrationThe reaction mixture is concentrated under reduced pressure and there
- concentrationReduced pressure concentration
- distillationto distill out the excess thionyl chloride completely
- distillationThe residue is distilled under reduced pressure
- customto collect a fraction boiling at 96°-8° C./2mmHg