反应详情

4-(2,3,4,5-Tetrahydro-1H-benzo[c]azepin-7-yloxymethyl)-benzoic acid methyl ester (D4) (2.83 g, 9.1 mmol) and cyclopentanone (1.6 ml, 18.2 mmol) were dissolved in dichloromethane (30 ml) and acetic acid (0.5 ml). Sodium triacetoxy borohydride (3.85 g, 18.2 mmol) was added and the solution was stirred at room temperature for 4 hours. The reaction mixture was washed with a saturated solution of sodium carbonate, the organic layer was dried over magnesium sulfate, filtered and concentrated in vacuo. The crude mixture was purified by column chromatography eluting with a mixture of 0.880 ammonia:ethanol:dichloromethane (1:9:90) to afford the title compound (E88); MS (ES+) m/e 380 [M+H]+.

1. washThe reaction mixture was washed with a saturated solution of sodium carbonate
2. dry with materialthe organic layer was dried over magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe crude mixture was purified by column chromatography
6. washeluting with a mixture of 0.880 ammonia:ethanol:dichloromethane (1:9:90)