反应详情

A mixture of 1-[3-(ethyloxy)-4-nitrophenyl]-4-[1-(2-fluoroethyl)-4-piperidinyl]piperazine (200 mg, 0.53 mmol) and platinum (sulfided, 5 wt. % on carbon, 50 mg, 0.013 mmol) in 20% MeOH/EtOAc (20 mL) was added to a high-pressure hydrogenation reaction flask. The reaction was purged with N2 and vacuum (3×). The reaction was purged with H2 and vacuum (3×). The reaction was then treated with H2 at 50 psi and stirred for approximately 16 h. The reaction was degassed, then poured through a Teflon filter, washing the solid with MeOH and DCM. The filtrate was concentrated under vacuum to give the title compound of step C (136 mg, 0.38 mmol, 74%) as a brown solid. MS (ESI): 351 [M+H]+.

1. additionwas added to a high-pressure hydrogenation reaction flask
2. customThe reaction was purged with N2 and vacuum (3×)
3. customThe reaction was purged with H2 and vacuum (3×)
4. additionThe reaction was then treated with H2 at 50 psi
5. customThe reaction was degassed
6. additionpoured through a Teflon
7. filtrationfilter
8. washwashing the solid with MeOH and DCM
9. concentrationThe filtrate was concentrated under vacuum