反应详情

温度

100 °C

2-Cyclohexylideneamino-benzoic acid (1.5 g, 6.9 mmol) was added to phosphorus oxychloride (4 mL) at 0° C. and stirred for 5 minutes followed by heating to 100° C. for 45 minutes. The reaction mixture was cooled to room temperature and slowly poured onto ice (˜100 g) and stirred for 30 minutes. CH2Cl2 (100 mL) was added and the mixture stirred for 5 minutes and the organic layer separated. The aq. layer was extracted with CH2Cl2 (50 mL). The combined CH2Cl2 layers were washed with sat. aq. NaHCO3 (2×50 mL), sat. aq. NaCl (50 mL), dried over Na2SO4, decanted and concentrated to give 9-chloro-1,2,3,4-tetrahydro-acridine, which, was used without further purification.

1. temperatureThe reaction mixture was cooled to room temperature
2. additionslowly poured onto ice (˜100 g)
3. stirringstirred for 30 minutes
4. stirringthe mixture stirred for 5 minutes
5. customthe organic layer separated
6. extractionThe aq. layer was extracted with CH2Cl2 (50 mL)
7. washThe combined CH2Cl2 layers were washed with sat. aq. NaHCO3 (2×50 mL), sat. aq. NaCl (50 mL)
8. dry with materialdried over Na2SO4
9. customdecanted
10. concentrationconcentrated