HRID357702

反应详情

EQUATION

反应方程式

HRID 357702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

132.2 g (1.00 mol) of tetralin was dissolved in 600 ml of 80% acetic acid, and 101.5 g (0.40 mol) of iodine, 45.5 g (0.20 mol) of periodic acid dihydrate and 15 ml of concentrated sulfuric acid were added thereto. The mixture was heated to 70° C. with stirring. The mixture was further stirred for 3 hours at the same temperature whereupon disappearance of tetralin was confirmed to terminate the reaction. The reaction mixture was added to 1000 ml of water, and the separated oily substance was extracted with 1000 ml of toluene. The toluene layer was washed with water and concentrated and then subjected to distillation under reduced pressure (bp: 120° C./3 mmHg) to obtain 215.3 g of the main fraction (yield: 83.4%). This product was a mixture of 5-iodotetralin and 6-iodotetralin in a blend ratio of 1:2.

WORKUP

后处理

  1. customto terminate
  2. customthe reaction
  3. extractionthe separated oily substance was extracted with 1000 ml of toluene
  4. washThe toluene layer was washed with water
  5. concentrationconcentrated
  6. distillationsubjected to distillation under reduced pressure (bp: 120° C./3 mmHg)
  7. customto obtain 215.3 g of the main fraction (yield: 83.4%)