反应详情

温度

35 °C

1-[3-(2-Hydroxyethyl)phenyl]-2-imidazolidinone was suspended in DMF (4 vol) and heated to 35° C. until a clear solution was obtained. Triethylamine (1 vol) was added dropwise at 30° C. over 15 minutes. The mixture was cooled to 20° C. and methanesulfonyl chloride (0.46 vol) was added 30 mins. The resulting suspension was stirred at 20° C. for 15 minutes. Dichloromethane (10 vol) was added, and the organic layer was washed with brine/water (1:1) (5 vol), and then water (3×5 vol). The organic phase was concentrated to 1 vol, and methanol was added (4 vol), if complete dissolution was not obtained, the mixture was heated to 35° C. in order to dissolve the solid. Methyl-t-butyl ether (10 vol) was added and the suspension was left to stand for 18 hours at room temperature. The suspension was filtered; the filter-cake was washed with methyl-t-butyl ether (2 vol). The solid was dried at 40° C. for 18 hours to give the title compound (70% th).

1. customwas obtained
2. temperatureThe mixture was cooled to 20° C.
3. washthe organic layer was washed with brine/water (1:1) (5 vol)
4. concentrationThe organic phase was concentrated to 1 vol, and methanol
5. additionwas added (4 vol)
6. dissolutionif complete dissolution
7. customwas not obtained
8. temperaturethe mixture was heated to 35° C. in order
9. dissolutionto dissolve the solid
10. waitthe suspension was left
11. waitto stand for 18 hours at room temperature
12. filtrationThe suspension was filtered
13. washthe filter-cake was washed with methyl-t-butyl ether (2 vol)
14. customThe solid was dried at 40° C. for 18 hours