反应详情

温度

85 °C

Into a 250-mL round-bottom flask equipped with a magnetic stir bar, a thermocouple, a condenser, and a nitrogen bubbler vented to a caustic scrubber, was charged 1-aminopropan-2-ol (60.0 g, 799 mmol). The mixture was heated to 85° C. and the product from Step A was added while maintaining the reaction temperature below 98° C. Upon completion of the addition the reaction mixture was stirred at 90 to 95° C. for 2.5 h. Chlorobenzene (50 mL) and water (25 mL) were added and the mixture was stirred at 70 to 75° C. for 15 min. The phases were allowed to separate and the lower organic phase was removed. The upper aqueous phase was extracted with chlorobenzene (2×25 mL) at 70 to 75° C. The combined organic phases were washed with water (2×25 mL) at 70 and 75° C. and 87.5 g of solvent was removed by distillation under reduced pressure at 60° C. (bath). The residue was diluted with chlorobenzene (125 mL). The resulting orange solution, which contained 0.032% water by Karl Fischer titration, was stirred overnight at 45° C. (bath).

1. customInto a 250-mL round-bottom flask equipped with a magnetic stir bar
2. temperaturewhile maintaining the reaction temperature below 98° C
3. additionUpon completion of the addition the reaction mixture
4. stirringthe mixture was stirred at 70 to 75° C. for 15 min
5. customto separate
6. customthe lower organic phase was removed
7. extractionThe upper aqueous phase was extracted with chlorobenzene (2×25 mL) at 70 to 75° C
8. washThe combined organic phases were washed with water (2×25 mL) at 70 and 75° C. and 87.5 g of solvent
9. customwas removed by distillation under reduced pressure at 60° C. (bath)
10. additionThe residue was diluted with chlorobenzene (125 mL)
11. stirringwas stirred overnight at 45° C. (bath)