反应详情

温度

40 °C

To a solution of (±)-(cis)-7-bromo-8,12-difluoro-1,3,4,14b-tetrahydro-2H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine (12.06 g, 31.65 mmol) in 120 mL of CH2Cl2, 25 mL of 2-propanol and 25 mL of ethanol at 40° C. was added a warm solution of (+)-phencyphos (3.84 g, 15.82 mmol) in 50 mL of CH2Cl2, 25 mL of 2-propanol and 25 mL of ethanol. The mixture was heated at 40° C., CH2Cl2 was carefully evaporated until a small amount of crystals was formed, and then the mixture was gradually cooled down to ambient temperature. The precipitate was filtered off and recrystallized to yield the title compound (3.94 g, 20%).

1. customCH2Cl2 was carefully evaporated until a small amount of crystals
2. customwas formed
3. temperaturethe mixture was gradually cooled down to ambient temperature
4. filtrationThe precipitate was filtered off
5. customrecrystallized