反应详情

1.00 g (2.67 mmol) of 2,2-bis(4-nitrobenzyl)malonic acid and 1.42 ml (10.7 mmol) 6-chlorohexanol were suspended in 5.0 ml toluene. 1.0 ml sulphuric acid are added. The reaction mixture was subsequently allowed to react for 21.5 hours at refluxing temperature. The reaction mixture was partitioned between water and ethyl acetate; the organic phase was washed repeatedly with water, dried over magnesium sulfate, filtered and concentrated by rotary evaporation. Chromatography of the residue on 150 g silica gel using toluene:ethyl acetate 19:1 as eluant yielded 0.94 g (78%) 6-chlorohexyl 2-(4-nitrobenzyl)-3-(4-nitrophenyl)propanoate as yellow oil.

1. customto react for 21.5 hours
2. temperatureat refluxing temperature
3. customThe reaction mixture was partitioned between water and ethyl acetate
4. washthe organic phase was washed repeatedly with water
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated by rotary evaporation