反应详情

89 g (1-benzyl-5-chloro-2,3,6,7-tetrahydro-1H-azepin-4-yl)-phenyl-methanol in 800 mL dichlormethane was dropped to 115.4 g pyridiniumchlorchromate in 600 mL dichlormethane. The reaction was stirred 2.5 days at RT. Potassiumcarbonate-solution was added to the reaction. The mixture was stirred 2 h at RT and filtered over celite. The layers were separated and the organic layer was washed with water. The solvent was removed and the residue was purified by chromatography on silica gel (toluol/EE: 8.5:1.5). The solvent was removed and 64.6 g of the desired compound was obtained. Rf: 0.5 (toluol/EE: 8.5:1.5)

1. stirringThe mixture was stirred 2 h at RT
2. filtrationfiltered over celite
3. customThe layers were separated
4. washthe organic layer was washed with water
5. customThe solvent was removed
6. customthe residue was purified by chromatography on silica gel (toluol/EE: 8.5:1.5)
7. customThe solvent was removed