反应详情

A suspension of 167d (4.0 g, 16 mmol) and Raney Ni (400 mg) in methanol (60 mL) was hydrogenated in a Parr apparatus at 50 psi overnight. The mixture was filtered through a pad of CELITE® and the filtrate was concentrated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with 20:1 methylene chloride/methanol to afford 167e as a yellow solid (2.0 g, 50%). MS: [M+H]+ 249.

1. customwas hydrogenated in a Parr apparatus at 50 psi overnight
2. filtrationThe mixture was filtered through a pad of CELITE®
3. concentrationthe filtrate was concentrated under reduced pressure
4. customThe residue was purified by silica-gel column chromatography
5. washeluting with 20:1 methylene chloride/methanol