反应详情

温度

20 °C

75.0 g (0.5 mol) of 5-aminobenzimidazolone and 41 g of anhydrous sodium acetate are initially introduced into 700 ml of N,N'-dimethylformamide and 776.8 g of 3-hydroxy-2-naphthoyl chloride (from 99.0 g (0.52 mol) of 3-hydroxy-2-naphthoic acid) in chlorobenzene are metered in at 5°-10° C. in the course of 30 min. After addition is complete, the mixture is subsequently stirred at 20° C. for 3 h, warmed to 50° C. and filtered. The filter cake does not filter off with suction very well (suction time: 14 h). For purification, the filter cake is taken up in 1 ml of methanol, the mixture is stirred and filtered off with suction, and the filter cake is washed with 250 ml of methanol and subsequently several times with a total of 1 l of boiling water. After drying, 130.3 g of 3-hydroxy-N-benzimidazolon-5-yl-2-naphthamide are obtained; this corresponds to 81.7% of theory.

1. customare metered in at 5°-10° C. in the course of 30 min
2. additionAfter addition
3. temperaturewarmed to 50° C.
4. filtrationfiltered
5. filtrationThe filter cake does not filter off with suction very well (suction time: 14 h)
6. customFor purification
7. stirringthe mixture is stirred
8. filtrationfiltered off with suction
9. washthe filter cake is washed with 250 ml of methanol and subsequently several times with a total of 1 l of boiling water
10. customAfter drying