反应详情

Diamide 3 (1.56 g) was added to diethyene glycol (25 mL). The reaction mixture was stirred at 175˜180° C. for 16 h. The brown solution was cooled to room temperature, and water was added (100 mL). The reaction mixture was extracted with a solvent consisting of ethyl acetate (80%) and t-butylmethyl ether (20%) (70 mL×7). The combined organic solvent was washed with water and brine, and dried over sodium sulfate. The solution was concentrated to approximately 20 mL. Anhydrous hydrogen chloride in ethyl acetate was added. The precipitate was filtered. The product was then dissolved in water (10 mL). The product was extracted with ethyl acetate (10 mL×6). Solvent was removed to afford diamine 4 as an off-white solid (767 mg).

1. extractionThe reaction mixture was extracted with a solvent
2. washThe combined organic solvent was washed with water and brine
3. dry with materialdried over sodium sulfate
4. concentrationThe solution was concentrated to approximately 20 mL
5. additionAnhydrous hydrogen chloride in ethyl acetate was added
6. filtrationThe precipitate was filtered
7. dissolutionThe product was then dissolved in water (10 mL)
8. extractionThe product was extracted with ethyl acetate (10 mL×6)
9. customSolvent was removed