反应详情

温度

70 °C

354 mg of palladium at a concentration of 10% on charcoal is added to 0.084 mole (23.1 g) of 4-chloro-2-(β-hydroxyethyl)amino-6-(β-hydroxyethyl)aminonitrobenzene in 23.7 g of triethylamine. 7 ml of formic acid are then run in dropwise. A high exothermicity is noted. The reaction mixture is heated to 70° C. for 1 hour 30. After dilution of the reaction mixture with ethanol, the catalyst is removed by hot filtration. The filtrate, evaporated to dryness under reduced pressure, enables a dry extract to be obtained. After dilution of the dry extract with water, the expected product precipitates. After being filtered off, washed with water and then dried under vacuum in the presence of phosphorus pentoxide, it is recrystallized twice from isopropanol. It melts at 103°-104° C., resolidifies and then melts at 112°-113° C.

1. customAfter dilution of the reaction mixture with ethanol, the catalyst is removed by hot filtration
2. customThe filtrate, evaporated to dryness under reduced pressure
3. extractionextract
4. customto be obtained
5. extractionAfter dilution of the dry extract with water
6. customthe expected product precipitates
7. filtrationAfter being filtered off
8. washwashed with water
9. dry with materialdried under vacuum in the presence of phosphorus pentoxide, it
10. customis recrystallized twice from isopropanol