反应详情

Water is decanted from wet Raney nickel (2.5 g) and toluene is added and additional water is azeotroped off under vacuum. Toluene and decalin (4 mL) are added to the damp Raney nickel and toluene is again azeotroped off. 1-Phenyl-1,2,9,10-tetrahydro[1,4]oxazino[2,3,4-jk]carbazol-7(8H)-one (0.180 g, 0.593 mmol) is added and the mixture is heated at 180° C. (additional toluene/water azeotroping occurs). After 3 h, the mixture is cooled. Dichloromethane is added and the Raney nickel is removed by filtration. The filtrate is concentrated under vacuum until solids begin precipitating out. Hexane is added and the mixture is stored in the refrigerator overnight. The solids are then collected by filtration (wash with hexane) and chromatographed on silica gel gel (30 mL) using ethyl acetate/hexane (20/80) to give 0.119 g (66%) of 1-phenyl-1,2-dihydro[1,4]oxazino[2,3,4-jk]carbazol-7-ol.

1. customWater is decanted from wet Raney nickel (2.5 g) and toluene
2. additionis added
3. customadditional water is azeotroped off under vacuum
4. additionToluene and decalin (4 mL) are added to the damp Raney nickel and toluene
5. customis again azeotroped off
6. temperaturethe mixture is cooled
7. customthe Raney nickel is removed by filtration
8. concentrationThe filtrate is concentrated under vacuum until solids
9. custombegin precipitating out
10. additionHexane is added
11. customis stored in the refrigerator overnight
12. filtrationThe solids are then collected by filtration (wash with hexane)
13. customchromatographed on silica gel gel (30 mL)