HRID47051

反应详情

EQUATION

反应方程式

HRID 47051 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.1 g (25 mM) of cyclopentanone, containing 0.3% of water, in 20 ml of THF were added dropwise to the reaction mixture while stirring. After having been left for two supplemental hours at reflux and stirring, the reaction mixture was cooled to room temperature, poured onto ice and extracted with ether. The combined organic extracts were successively washed with 1N HCl, a diluted aqueous solution of sodium bicarbonate and finally water. By the evaporation of the volatile components there were obtained 3.7 g of residue which, upon bulb-distillation gave 2.25 g (yield 67%) of the desired spiro-heptanone having a b.p. of 110°-125°/10 Torr. The assessed purity is of about 90%. The product represents an isomeric mixture containing cis- and trans- 1-(prop-1-en-1-yl) spiro [2.4]heptan-4-one in a 2:1 respective weight ratio.

WORKUP

后处理

  1. waitAfter having been left for two supplemental hours
  2. temperatureat reflux
  3. stirringstirring
  4. additionpoured onto ice
  5. extractionextracted with ether
  6. washThe combined organic extracts were successively washed with 1N HCl
  7. customBy the evaporation of the volatile components