反応 #444884

反応方程式

5-iodotetralin

6-iodotetralin

iodine

periodic acid dihydrate

sulfuric acid

tetralin

tetralin

→

iodotetralin

収率 83.4%

溶媒

water

acetic acid

反応条件

後処理

1. 1
   その他to terminate
2. 2
   その他the reaction
3. 3
   抽出the separated oily substance was extracted with 1000 ml of toluene
4. 4
   洗浄The toluene layer was washed with water
5. 5
   濃縮concentrated
6. 6
   workup.DISTILLATIONsubjected to distillation under reduced pressure (bp: 120° C./3 mmHg)
7. 7
   その他to obtain 215.3 g of the main fraction (yield: 83.4%)

実験手順

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.

出典