反应详情

温度

80 °C

The compound, toluene-4-sulphonic acid-3-(2-methoxy-5-methylphenyl)-3-phenylpropyl ester (prepared as described in EP 0325571, 1.5 gm, 3.66 mmole, 1 eq) was dissolved in dry acetonitrile (4 ml). To the reaction mixture, 3-benzyl-3,6-diazabicyclo[3.1.0]hex-6-yl amine, 1.38 gm, 7.32 mmole, 2 eq, (prepared according to T. F. Braish et al. Synlett 1996, 1100) and triethylamine (5.1 ml) were added. The resulting reaction mixture was heated at 80° C. for 4 days. The solvents were evaporated off, from the reaction mixture under reduced pressure. The residue was dissolved in ethyl acetate, and washed with saturated sodium bicarbonate solution. The organic layer was separated, dried over sodium sulphate and concentrated under high vaccum. The crude compound was purified through column chromatography using ethyl acetate in hexane solvent system.

1. additionwere added
2. customThe resulting reaction mixture
3. customThe solvents were evaporated off, from the reaction mixture under reduced pressure
4. dissolutionThe residue was dissolved in ethyl acetate
5. washwashed with saturated sodium bicarbonate solution
6. customThe organic layer was separated
7. dry with materialdried over sodium sulphate
8. concentrationconcentrated under high vaccum
9. customThe crude compound was purified through column chromatography