反应详情

A mixture of 5 g 5% palladium-carbon, 2.8 liters of methanol, 59 g of potassium acetate (anhydride), and 138.4 g methyl 5-chloro-3-nitroanthranilate was subjected to hydrogen absorption with stirring and cooling with a water bath. When the hydrogen absorption was completed, the reaction mixture was filtered, and the filtrate was concentrated in vacuo. To the residue were added ice and 1 lit mixture of n-hexane:ethyl acetate (6:4) and separated. The organic solvent layer was washed with saturated sodium bicarbonate solution, then washed with saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated in vacuo to give dark brown crystals, m.p. 59°-61° C.

1. customwas subjected to hydrogen absorption
2. temperaturecooling with a water bath
3. customWhen the hydrogen absorption
4. filtrationthe reaction mixture was filtered
5. concentrationthe filtrate was concentrated in vacuo
6. additionTo the residue were added ice and 1
7. additionmixture of n-hexane:ethyl acetate (6:4)
8. customseparated
9. washThe organic solvent layer was washed with saturated sodium bicarbonate solution
10. washwashed with saturated sodium chloride solution
11. dry with materialdried with anhydrous magnesium sulfate
12. concentrationconcentrated in vacuo
13. customto give dark brown crystals, m.p. 59°-61° C.