反应详情

To a solution of crude 1-benzyl-4-hydroxy-4-aminomethyl piperidine, as described above in Step A, (˜3.1 gm, 12 mmol) in acetonitrile (50 mL) containing triethyl amine (5.7 mL, 42 mmol) cooled in an ice bath was added in 1 mL portions 20% phosgene/toluene (9 mL) over a three hour period. The reaction mixture was stirred at ambient temp. for 15 hours and diluted with ethyl acetate. This solution was washed with water (2×) and the organic layer dried (anhyd. sodium sulfate), filtered, and the solvent removed under vacuum. The residue was triturated with diethyl ether and the title compound collected by filtration as a white solid, mp: 159-161° C.

1. temperaturecooled in an ice bath
2. washThis solution was washed with water (2×)
3. dry with materialthe organic layer dried (anhyd. sodium sulfate)
4. filtrationfiltered
5. customthe solvent removed under vacuum
6. customThe residue was triturated with diethyl ether
7. filtrationthe title compound collected by filtration as a white solid, mp: 159-161° C.