反应详情

温度

60 °C

13.7 g (42.0 mmol) of cesium carbonate and 3.24 g (11.56 mmol) of 4-(t-butyloxycarbonylamino)butyl bromide were added to a solution of 4.0 g (10.51 mmol) of diethyl 2-[1-(toluene-4-sulfonyl)-1H-imidazol-4-yl]malonate in 67 ml of DMF, and the mixture was stirred at 60° C. for 2 h. The reaction mixture was concentrated under reduced pressure, and the residue was taken up in ethyl acetate and washed with water. The organic phase was dried over Na2SO4, filtered and concentrated. Chromatography on silica gel (heptane/ethyl acetate 1:1) gave the title compound (4.21 g, 73%). LC/MS: Rt=2.08 min, [M+H]+=552, (method A).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. washwashed with water
3. dry with materialThe organic phase was dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated