HRID1763390

反应详情

EQUATION

反应方程式

HRID 1763390 的结构方程式

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

  1. stirringunder stirring
  2. customto remove excess bromine
  3. extractionThe aqueous solution is extracted twice
  4. dry with materialeach time with 20 ml of carbon tetrachloride, and the combined extracts are dried with magnesium sulfate
  5. distillationCarbon tetrachloride is distilled out
  6. distillationthe residue (1.9 g) is distilled under reduced pressure
  7. customto collect a fraction boiling at 96°-8° C/2mmHg