HRID280424

反应详情

EQUATION

反应方程式

HRID 280424 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a three-necked vessel of 250 ml equipped with a thermometer, a condenser and a dropping funnel, there were placed 23.9 g (0.427M) of finely ground KOH and 50 ml of anhydrous diethyl ether. 14 G (0.1M) of 2,6,6-trimethylcyclohexanone and 13.5 g (0.138M) of hex-1-yn-3-ol were then added dropwise to the obtained suspension. The addition is slightly exothermic. After standing for 24 h, the mixture was poured onto ice and extracted with ether while the combined extracts were washed with a 10% HCl solution, with brine until neutrality and finally dried over Na2SO4 and concentrated. A fractional distillation of the obtained residue gave 12 g of 1-(1-hydroxy-2,6,6-trimethylcyclohexyl)-hex-1-yn-3-ol having b.p. 100°-125°/13.3 Pa.

WORKUP

后处理

  1. customIn a three-necked vessel of 250 ml equipped with a thermometer, a condenser and a dropping funnel, there
  2. additionThe addition
  3. additionthe mixture was poured onto ice
  4. extractionextracted with ether while the combined extracts
  5. washwere washed with a 10% HCl solution, with brine until neutrality
  6. dry with materialfinally dried over Na2SO4
  7. concentrationconcentrated
  8. distillationA fractional distillation of the obtained residue