HRID482137

反应详情

EQUATION

反应方程式

HRID 482137 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

In a 300-ml three-necked flask equipped with a water separator, 70 g (1 mole) of crotonaldehyde, 144 g (2 mole) of crotyl alcohol, 3 mg of stannous chloride dihydrate and 40 g of hexane were charged. The resulting mixture was heated at 70° C. under atmospheric pressure and for 4 hours in a nitrogen atmosphere while removing the water formed from the reaction mixture by azeotropic distillation. When water was no longer distilled, the solvent (hexane) and unreacted starting materials were distilled off under reduced pressure. Distillation of the residue under reduced pressure gave 182.2 g of crotonaldehyde dicrotyl acetal [R1 =a 1-propenyl group, R2 =a hydrogen atom and R3 =a crotyl group) (boiling point: 120° C./25 mmHg) (yield: 91.9%).

WORKUP

后处理

  1. additionwere charged
  2. customwhile removing the water
  3. customformed from the reaction mixture by azeotropic distillation
  4. distillationWhen water was no longer distilled
  5. distillationwere distilled off under reduced pressure
  6. distillationDistillation of the residue under reduced pressure