HRID1032503

反应详情

EQUATION

反应方程式

HRID 1032503 的结构方程式

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a stirred mixture of 6.01 g of 4-(2-furyl)-1-butyne [Perfumery Essent. Oil Record., 57, 364 (1966)], 10.6 g of sodium carbonate and 150 ml of methanol at -25° C., was added dropwise a solution of 8.0 g of bromine in 50 ml of methanol during a period of 3 hours. The mixture was then stirred at 25° C. for 45 minutes and concentrated in vacuo. The residue was partitioned with ether and brine. The ether layer was separated, washed with brine, dried and concentrated. Distillation of the residue at 0.5mm gave 6.62 g of the desired compound as a light yellow liquid, bp 57°-61° C. (0.5 mm).

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. customThe residue was partitioned with ether and brine
  3. customThe ether layer was separated
  4. washwashed with brine
  5. customdried
  6. concentrationconcentrated
  7. distillationDistillation of the residue at 0.5mm