反应详情

To a mixture of 5 g (0.033 mol) of 3,5-diaminobenzoic acid in 100 ml of methylene chloride, 50 ml of THF and 18 ml (0.13 mol) of triethylamine stirred at room temperature was added 17 ml (0.08 mol) of decanoyl chloride dropwise over 10 minutes. The reaction mixture was stirred for 18 hours, filtered and the filtrate was concentrated at reduced pressure. Water was added to the residue and the product was extracted with ethyl acetate. The dried extract was concentrated at reduced pressure and the solid residue was recrystallized twice from methanol-water to give 8.6 g (57% yield, mp 208°-209°) of 3,5-bis[(1-oxodecyl)amino]benzoic acid.

1. stirringThe reaction mixture was stirred for 18 hours
2. filtrationfiltered
3. concentrationthe filtrate was concentrated at reduced pressure
4. additionWater was added to the residue
5. extractionthe product was extracted with ethyl acetate
6. extractionThe dried extract
7. concentrationwas concentrated at reduced pressure
8. customthe solid residue was recrystallized twice from methanol-water