反应详情

温度

-10 °C

To a cooled (−10° C.) solution of thiocarbonyldiimidazole (211 g, 1.178 mol) in THF (1.5 L) was added slowly via cannula a solution of N′-(4-amino-2-cyanophenyl)-N,N-dimethylformamidine (201.6 g, 1.071 mol) in THF (1.5 L). After stirring at −10° C. for 25 minutes, a solution of 2-amino-2-methylpropan-1-ol (120 g, 1.4 mol) in THF (500 mL) was slowly added to the mixture. After warming to room temperature and stirring for 16 hours, the mixture was washed with saturated sodium chloride (2×2 L). The combined aqueous layers were extracted with MTBE (2 L) and ethyl acetate (4×1 L). The combined organic layers were dried over MgSO4 and concentrated under reduced pressure. The residue was crystallized with MTBE and ethyl acetate to provide the product (116.9 g, 34%) as yellow solid.

1. temperatureAfter warming to room temperature
2. stirringstirring for 16 hours
3. washthe mixture was washed with saturated sodium chloride (2×2 L)
4. extractionThe combined aqueous layers were extracted with MTBE (2 L) and ethyl acetate (4×1 L)
5. dry with materialThe combined organic layers were dried over MgSO4
6. concentrationconcentrated under reduced pressure
7. customThe residue was crystallized with MTBE and ethyl acetate