反应详情

Combine 1-(3,4,5-trimethoxybenzoyl)-3-(3,4-dichlorophenyl)-3-(2-methanesulfonyloxyethyl)piperidine (0.71 g, 1.32 mmol) and 4-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl)[1,4]diazepane (0.38 g, 1.32 mmol), and N,N-diisopropylethylamine (0.37 g, 2.9 mmol) in acetonitrile (15 mL). Heat to reflux. After 36 hours, partition the residue between ethyl acetate and saturated aqueous sodium bicarbonate solution. Dry the organic layer over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Chromatograph the residue on silica gel eluting with 15% methanol/2% triethylamine/ethyl acetate to give the title compound. Elemental Analysis calculated for C39H49Cl2N5O5: C 63.40; H 6.68; N 9.48; Found: C 63.68; H 6.69; N 9.57.

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