反应详情

温度

60 °C

A solution of ethyl(4-aminophenyl)acetate (1.76 g, 9.84 mmol) and acetic acid (0.71 ml) in DMF (71 ml) is added to a solution of 2-heptyloxy-4-iodobenzaldehyde of Step c (3.1 g, 8.94 mmol), acetic acid (0.71 ml) in DMF (71 ml). The mixture is stirred for 12 hours and then 1.12 g of sodium cyanoborohydride (17.89 mmol) is added. The mixture is heated at 60° C. for 4 hours. The desired product is extracted by addition of ethyl ether. The organic phase is washed with brine and then with water, dried with magnesium sulfate and concentrated using a rotary evaporator. The product is purified by chromatography on a silica column, eluted with a heptane/ethyl acetate 9:1 mixture. After evaporation of the solvents, 4.11 g (96%) of the expected compound are recovered in the form of a yellow oil.

1. extractionThe desired product is extracted by addition of ethyl ether
2. washThe organic phase is washed with brine
3. dry with materialwith water, dried with magnesium sulfate
4. concentrationconcentrated
5. customa rotary evaporator
6. customThe product is purified by chromatography on a silica column
7. washeluted with a heptane/ethyl acetate 9:1 mixture
8. customAfter evaporation of the solvents, 4.11 g (96%) of the expected compound
9. customare recovered in the form of a yellow oil