HRID1112184

反应详情

EQUATION

反应方程式

HRID 1112184 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 entirety 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 decompose excess bromine. The aqueous solution is subjected to two extractions each 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. Colorless crystals having a melting point of 57.5°-58.5° C. are thus obtained.

WORKUP

后处理

  1. stirringunder stirring
  2. extractionThe aqueous solution is subjected to two extractions each with 20 ml of carbon tetrachloride
  3. dry with materialthe combined extracts are dried with magnesium sulfate
  4. distillationCarbon tetrachloride is distilled out
  5. distillationthe residue (1.9 g) is distilled under reduced pressure
  6. customto collect a fraction boiling at 96°-8° C./2mmHg
  7. customare thus obtained