反应详情

The 4-methyl-4-nitropentanoic acid (4.3 g) obtained above was dissolved in dichloromethane, and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (6.1 g) and triethylamine (4.5 ml) were added thereto and stirred for 1 hour. Benzylamine (3.4 g) was added thereto and stirred for 1 day. Water was added to the reaction mixture which was then acidified by 2 N hydrochloric acid and extracted with chloroform. The organic phase was washed with a saturated sodium bicarbonate solution and a saturated saline solution and dried over sodium sulfate anhydrous. The resulting product was concentrated under reduced pressure, and the residue was purified by column chromatography (eluting solvent; ethyl acetate:n-hexane 1:1.5) to give N-benzyl-4-methyl-4-nitropentanoic acid amide (2.5 g, Y.:38%) as a colorless oil.

1. stirringstirred for 1 day
2. extractionextracted with chloroform
3. washThe organic phase was washed with a saturated sodium bicarbonate solution
4. dry with materiala saturated saline solution and dried over sodium sulfate anhydrous
5. concentrationThe resulting product was concentrated under reduced pressure
6. customthe residue was purified by column chromatography (eluting solvent; ethyl acetate:n-hexane 1:1.5)