反应详情

温度

90 °C

A solution of N-(2,6-dichloro-4-nitrophenyl)-3-cyclopentyloxy-4-methoxybenzamide (1.5 g) in glacial acetic acid (22 mL) is treated with iron pin dust (1.3 g) and the mixture is heated with stirring at 90° C. for 1 hour. The reaction mixture is cooled, basified to pH 8 by treatment with saturated aqueous sodium carbonate solution, and extracted with ethyl acetate (2×150 mL). The combined organic extract is dried over magnesium sulfate and concentrated in vacuo, to give a white solid. This solid is subjected to flash chromatography, eluting with a mixture of ethyl acetate and pentane (1:1 v/v), to give N-(2,6-dichloro-4-aminophenyl)-3-cyclopentyloxy-4-methoxybenzamide (0.8 g), m.p. 170-172° C. [Elemental analysis: C, 54.8; H, 5.04; N, 6.5; Cl, 17.4%; calculated: C, 57.7; H, 5.1; N, 7.1; Cl, 17.9%].

1. temperaturethe mixture is heated
2. temperatureThe reaction mixture is cooled
3. extractionextracted with ethyl acetate (2×150 mL)
4. extractionThe combined organic extract
5. dry with materialis dried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. customto give a white solid
8. washeluting with a mixture of ethyl acetate and pentane (1:1 v/v)