反应详情

N-Benzyl-5-(4-methylpiperazin-1-yl)-2-nitroaniline E-1.1′ (5.000 g; 15.319 mmol) is dissolved in THF (50.000 ml) and filled into a Büchi autoclave. RaNi (500.000 mg) is added and hydrogenated at 6 bar overnight (pressure after 16 h=0.5 bar). The autoclave is filled again with 6 bar H2 and stirred for 5 hours at rt. The reaction mixture is filtered through a plug of celite and HCl in dioxane (4 M, 4.000 ml; 16.000 mmol) is added. The filtrate is concentrated under reduced pressure to give a residue, which is dissolved in the smallest possible amount of MeOH and sonicated for few minutes. Precipitation of the product occurs and the product is filtered off. The product is washed with a very small amount of MeOH and 50 ml of isopropyl ether and then dried under reduced pressure.

1. additionfilled into a Büchi autoclave
2. customhydrogenated at 6 bar overnight (pressure after 16 h=0.5 bar)
3. additionThe autoclave is filled again with 6 bar H2
4. additionis added
5. concentrationThe filtrate is concentrated under reduced pressure
6. customto give a residue, which
7. customsonicated for few minutes
8. customPrecipitation of the product
9. filtrationthe product is filtered off
10. washThe product is washed with a very small amount of MeOH and 50 ml of isopropyl ether
11. customdried under reduced pressure