反应详情

8.8 g of 1,4-cyclohexanedione was dissolved with 40 mL of methanol. Solution was cooled to 10C and 4.2 mL of bromine was dropwise added at this temperature during 15 minutes. The temperature was kept at 10C for one hour and then allowed to rise to 20C. When bromine colour faded, 7.2 g of thiourea was added. The reaction mixture was then diluted with 20 mL of water and heated under reflux for 2 h. White precipitate was removed by filtration and filtrate was concentrated in vacuo and cooled. The crystals of product (6) were filtered off and washed with a cold water.

1. additionwas dropwise added at this temperature during 15 minutes
2. temperatureheated
3. temperatureunder reflux for 2 h
4. customWhite precipitate was removed by filtration and filtrate
5. concentrationwas concentrated in vacuo
6. temperaturecooled
7. filtrationThe crystals of product (6) were filtered off
8. washwashed with a cold water