反应详情

To a solution of 2-(2-nitro-5-chlorophenylmethyl) benzoic acid methyl ester (840 mg; prepared in reference example 3) in a mixture of acetic acid-water (5:1; 12 ml) was added steel powder (768 mg) and the mixture was added for 20 minutes at 80° C. The suspension was poured into ice-water and was extracted with ethyl acetate. The organic layer was washed with water, a saturated aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride successively, dried, and was concentrated. The residue was purified by column chromatography on silica gel to give the title compound (363 mg) having the following physical data.

1. additionthe mixture was added for 20 minutes at 80° C
2. extractionwas extracted with ethyl acetate
3. washThe organic layer was washed with water
4. dry with materiala saturated aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride successively, dried
5. concentrationwas concentrated
6. customThe residue was purified by column chromatography on silica gel