反应详情

温度

90 °C

After heating to 90° C. a mixture of 38.68 g of (+)-cis-1,3-dibenzylhexahydrofuro[3,4-d]imidazole-2,4-dione, 6.04 g of sodium acetate, 2.49 g of sulfur and 47.56 g of polyethylene glycol (the average molecular weight: 600), it was stirred for 4.5 hours at the temperature while blowing 4.50 g of hydrogen sulfide at a rate of 10 ml/minute. Then blowing of hydrogen sulfide was stopped and the resultant mixture was stirred for 5 hours at the temperature. After cooling the reaction mixture to room temperature, 173.61 g of toluene and 99.70 g of water were added to the mixture, and 8.25 g of zinc powder was further added to the mixture while stirring at room temperature. After dropping 54.90 g of 35% hydrochloric acid at the same temperature, the resultant mixture was stirred at 45° C. for 8 hours. The mixture was separated by removing water layer to give an oil layer, which was concentrated to give a product. Recrystallization from 2-propanol and water gave a crystal of (+)-cis-1,3-dibenzylhexahydrothieno[3,4-d]imidazole-2,4-dione. The yield was 36.96 g (yield percentage: 91%). Melting point was 126° C. [α]D20 was 90° C.=1.0; chloroform).

1. temperatureAfter cooling the reaction mixture to room temperature
2. additionwas further added to the mixture
3. stirringwhile stirring at room temperature
4. customThe mixture was separated
5. customby removing water layer
6. customto give an oil layer, which
7. concentrationwas concentrated
8. customto give a product
9. customRecrystallization from 2-propanol and water