反应详情

To a stirred solution of 10 (R8═C4H2N2Cl, R2═COCF3; 614 mg, 1.26 mmol) in THF (50 mL) and ammonia (22 mL), zinc (2.17 g 33.2 mmol) was added. The reaction mixture was stirred for 5 hours under reflux. The reaction was quenched with a saturated NaHCO3 solution in H2O and filtered over decalite. The product was extracted into ethyl acetate, washed with brine, dried (Na2SO4) and concentrated under reduced pressure. The crude product was purified by column chromatography on silica affording rel-2,2,2-trifluoro-N-[(2R,10R,14bR)-1,2,3,4,10,14b-hexahydro-10-methyl-8-(pyrimidin-4-yl)dibenzo[c,f]pyrido[1,2-a]azepin-2-yl]acetamide (10: R8═C4H3N2, R2═COCF3; 485 mg, 85%). Data: (m/z)=453 (M+H)+.

1. temperatureunder reflux
2. customThe reaction was quenched with a saturated NaHCO3 solution in H2O
3. filtrationfiltered over decalite
4. extractionThe product was extracted into ethyl acetate
5. washwashed with brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated under reduced pressure
8. customThe crude product was purified by column chromatography on silica