Ammonia → Ammonia

0.88 Ammonia (85 ml) was added to a solution of N-acetylpiperidone (15 g, 106 mmol) in methanol (120 ml), followed by palladium hydroxide (2 g) and the mixture hydrogenated at room temperature and 60 psi for 18 hours. The reaction mixture was filtered through Arbocel®, the filtrate concentrated under reduced pressure and the residue azeotroped with toluene to give a yellow oil. The crude product was purified by column chromatography on silica gel using an elution gradient of dichloromethane:methanol:0.88 ammonia (96:3.5:0.5 to 84:14:2) to afford the title compound as a clear oil, 9.6 g.

1. filtrationThe reaction mixture was filtered through Arbocel®
2. concentrationthe filtrate concentrated under reduced pressure
3. customthe residue azeotroped with toluene
4. customto give a yellow oil
5. customThe crude product was purified by column chromatography on silica gel using an elution gradient of dichloromethane

ORDレコード

ord-3aeb0bdf566a4404b998247c8e514b62

出典データセット

uspto-grants-2006_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07060836B2