反应详情

温度

65 °C

Subsequently, ammonium chloride (0.9 g) and iron powder (4.5 g) were added to a mixed solvent of water (10 ml) and ethanol (30 ml), and the mixture was heated to 65° C. Then, 2-bis(2-hydroxyethyl)amino-5-nitrobenzonitrile (11 g) was added in parts over 20 min and the mixture was stirred at a refluxing temperature for 30 min. The reaction mixture was ice-cooled and filtrated. The solvent was evaporated under reduced pressure. To the residue was added aqueous sodium hydroxide ice solution and the mixture was extracted with toluene. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate, after which the solvent was evaporated under reduced pressure. n-Hexane was added to the residue to allow crystallization. The crystals were recrystallized from a mixed solvent of diisopropyl ether-n-hexane to give the title compound (8 g), melting point: 38° C.

1. temperaturecooled
2. filtrationfiltrated
3. customThe solvent was evaporated under reduced pressure
4. additionTo the residue was added aqueous sodium hydroxide ice solution
5. extractionthe mixture was extracted with toluene
6. washThe organic layer was washed with saturated brine
7. dry with materialdried over anhydrous sodium sulfate
8. customafter which the solvent was evaporated under reduced pressure
9. additionn-Hexane was added to the residue
10. customcrystallization
11. customThe crystals were recrystallized from a mixed solvent of diisopropyl ether-n-hexane