反应详情

Dissolve 7-chloro-3-(2,2,2-trifluoroacetyl)-6-[3-(2-phenyl-[1,3]dioxolan-2-yl)-propylamino]-2,3,4,5-tetrahydro-1H-benzo[d]azepine (2.78 g, 5.76 mmol) in DCM (25 mL) and add methanol (1 mL) and 2 N HCl in diethyl ether (25 mL) and stir at RT for 16 h. Concentrate and dissolve the residue in acetic acid (30 mL) and add sodium cyanoborohydride (1.81 g, 28.78 mmol). Stir the reaction at RT for 1 h then concentrate. Dissolve the residue in EtOAc (500 mL) and extract with saturated sodium bicarbonate solution (500 mL). Extract the aqueous layer with EtOAc (100 mL) and combine the organic fractions, dry (sodium sulfate), concentrate and purify (silica gel chromatography, eluting with 10:90 EtOAc:hexanes) to give the title compound as a foam (1.72 g, 71%).

1. concentrationConcentrate
2. dissolutiondissolve the residue in acetic acid (30 mL)
3. stirringStir
4. customthe reaction at RT for 1 h
5. concentrationthen concentrate
6. dissolutionDissolve the residue in EtOAc (500 mL)
7. extractionextract with saturated sodium bicarbonate solution (500 mL)
8. extractionExtract the aqueous layer with EtOAc (100 mL)
9. dry with materialdry (sodium sulfate)
10. concentrationconcentrate
11. custompurify
12. wash(silica gel chromatography, eluting with 10:90 EtOAc:hexanes)