反应详情

To a solution of 0.70 g of N-[2-bromo-4-[3-(3,5-dichlorophenyl)-4,4,4-trifluoro-3-(nitromethyl) butanoyl]phenylmethyl]phthalimide and 1.03 g of ammonium formate in 20 mL of tetrahydrofuran, 1.07 g of zinc powder was added and the resultant reaction mixture was stirred while heating the mixture to reflux for 1 hour. After the completion of the reaction, the reaction mixture was left to be cooled down to room temperature, and 100 mL of ethyl acetate and 50 mL of water were added to the reaction mixture, followed by filtering the reaction mixture with Celite. Subsequently, the organic phase was separated off and was dehydrated and dried over a saturated brine and anhydrous magnesium sulfate in this order, and the solvent was distilled off under reduced pressure. The resultant residue was purified by silica gel column chromatography eluting with chloroform to obtain 0.18 g of the objective substance as a white crystal.

1. customthe resultant reaction mixture
2. temperaturewhile heating the mixture
3. temperatureto reflux for 1 hour
4. customAfter the completion of the reaction
5. waitthe reaction mixture was left
6. filtrationby filtering the reaction mixture with Celite
7. customSubsequently, the organic phase was separated off
8. dry with materialdried over a saturated brine and anhydrous magnesium sulfate in this order
9. distillationthe solvent was distilled off under reduced pressure
10. customThe resultant residue was purified by silica gel column chromatography
11. washeluting with chloroform
12. customto obtain 0.18 g of the objective substance as a white crystal