反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
1.0 Gram (4.8 millimoles) of tricyclo [4.3.1.12,5 ] undecane is added to 2 ml (38.7 millimoles) of liquid bromine and the whole is stirred at room temperature for 17 hours. The reaction mixture is added slowly to a cooled saturated solution of sodium hydrogensulfite under stirring to remove excess bromine. The aqueous solution is extracted twice, each time with 20 ml of carbon tetrachloride, and the combined extracts are dried with magnesium sulfate. Carbon tetrachloride is distilled out and the residue (1.9 g) is distilled under reduced pressure to collect a fraction boiling at 96°-8° C/2mmHg to obtain 1.0 g (yield 65.5%) of 1-bromotricyclo [4.3.1.12,5 ] undecane. Upon cooling, white crystals of a melting point of 57.5° to 58.5° C are obtained.
WORKUP
后处理
- stirringunder stirring
- customto remove excess bromine
- extractionThe aqueous solution is extracted twice
- dry with materialeach time with 20 ml of carbon tetrachloride, and the combined extracts are dried with magnesium sulfate
- distillationCarbon tetrachloride is distilled out
- distillationthe residue (1.9 g) is distilled under reduced pressure
- customto collect a fraction boiling at 96°-8° C/2mmHg