反应详情

Combine 1-(3,4,5-trimethoxybenzoyl)-3-(3,4-dichlorophenyl)-3-(2-methanesulfonyloxyethyl)piperidine (1.14 mmol) and (1-(4-fluorobenzyl)-1H-benzimidazol-2-yl)(piperidin-4-yl)amine (0.56 g, 1.7 mmol), and N,N-diisopropylethylamine (0.50 g) in acetonitrile (12 mL). Heat to reflux. After 2 days, partition the residue between ethyl acetate and water. Separate the organic layer and extract twice with saturated aqueous sodium bicarbonate solution and brine. Dry the organic layer over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Chromatograph the residue on silica gel eluting with 30/70/0.33 methanol/ethyl acetate/concentrated aqueous ammonia to give the title compound: Rf=0.50 (silica gel, 30% methanol/ethyl acetate).

1. temperatureHeat to reflux
2. custompartition the residue between ethyl acetate and water
3. customSeparate the organic layer
4. extractionextract twice with saturated aqueous sodium bicarbonate solution and brine
5. dry with materialDry the organic layer over Na2SO4
6. filtrationfilter
7. concentrationconcentrate in vacuo
8. customto obtain a residue