反应详情

温度

5 °C

To a mixture of 24.9 g (90.9 mmol) of 6-tert-butyl-2-isobutyl-5-methoxyindan-1-one, 25.8 g of potassium acetate, 0.5 g of Et4NI, 50 ml of dichloromethane and 150 ml of water 4.66 ml (14.5 g, 90.9 mmol) of bromine was added dropwise by vigorous stirring at 5° C. for 5 min. This mixture was stirred at 5° C. for 3 h, then 15.2 g of potassium acetate was added, and finally 2.56 ml (8.24 g, 51.6 mmol) of bromine was added. The resulting mixture was additionally stirred at this temperature for 1 h. and then washed by aqueous Na2SO3 to remove an excess of bromine. The product was extracted by 3×150 ml of dichloromethane, The combined organic extract was dried over K2CO3, evaporated to dryness, and the residue was dried in vacuum. This procedure gave 31.9 g (99%) of yellowish crystalline material which was further used without an additional purification.

1. additionwas added dropwise
2. stirringThis mixture was stirred at 5° C. for 3 h
3. stirringThe resulting mixture was additionally stirred at this temperature for 1 h.
4. washwashed by aqueous Na2SO3
5. customto remove an excess of bromine
6. extractionThe product was extracted by 3×150 ml of dichloromethane
7. extractionThe combined organic extract
8. dry with materialwas dried over K2CO3
9. customevaporated to dryness
10. customthe residue was dried in vacuum