反应详情

To a mixture of 3-benzyloxy-N-methyl-2-nitroaniline (453.3 mg), 80% methanol (6.8 ml), anhydrous ferric chloride (13.6 mg) and carbon (13.6 mg) was dropwise added hydrazine monohydrate (255.6 μl) at 70° C., and the mixture was stirred for 5 hours at the same temperature. Insoluble material was filtered off, and the filtrate was concentrated in vacuo. Ethyl acetate and saturated sodium bicarbonate solution were added to the residue, and the organic layer was washed with water and brine, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel (ethyl acetate-n-hexane) to give 2-amino-3-benzyloxy-N-methylaniline (348.9 mg).

1. customat 70° C.
2. filtrationInsoluble material was filtered off
3. concentrationthe filtrate was concentrated in vacuo
4. additionEthyl acetate and saturated sodium bicarbonate solution were added to the residue
5. washthe organic layer was washed with water and brine
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated in vacuo
8. customThe residue was purified by column chromatography on silica gel (ethyl acetate-n-hexane)