HRID436388

反应详情

EQUATION

反应方程式

HRID 436388 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

cyclotridecanone: 200 ml of a 50 % aqueous solution of NaOH were added dropwise under vigorous stirring to a mixture of 132 g of cyclododecene (CHEMICAL SAMPLE Co - Columbus, Ohio - USA), 600 g of bromoform and 4 g of tetramethylammonium bromide. The mixture was then left at a temperature between 40° and 50° under stirring during 2 h, whereupon it was left at room temperature overnight and diluted with water. Finally the reaction mixture was extracted with 3 fractions of 300 ml each of ether. The combined extracts, after the usual treatments of washing, drying and evaporation, gave a residue which upon fractional distillation under reduced pressure yielded 173 g (92 %) of 2,2-dibromo-bicyclo[10.1.0]tridecane.

WORKUP

后处理

  1. waitThe mixture was then left at a temperature between 40° and 50°
  2. waitwas left at room temperature overnight
  3. extractionFinally the reaction mixture was extracted with 3 fractions of 300 ml each of ether
  4. washThe combined extracts, after the usual treatments of washing
  5. customdrying
  6. customevaporation
  7. customgave a residue which
  8. distillationupon fractional distillation under reduced pressure