反应详情

To a solution of 4-(2-aminophenylamino)benzophenone (Compound 101. 0.29 g, 1mmol) and O-methylhydroxylamine hydrochloride (0.30 g, 3.5 mmol) in ethanol (10 ml) was added sodium acetate (0.30 g, 4 mmol). The reaction mixture was refluxed for 25 hours, cooled to room temperature, filtered, and evaporated in vacuo. The residue was treated with diluted ammonium hydroxide (10 ml) and extracted with ethyl acetate (2×25 ml). The organic phase was dried (MgSO4), filtered and evaporated in vacuo. The residue was dissolved in diethyl ether and acidified with hydrochloric acid in diethyl ether. The hydrochloride of the title compound instantaneously precipitate. The precipitate was triturated with ethyl acetate and washed with diethyl ether to yield the title compound as a hydrochloride.

1. temperatureThe reaction mixture was refluxed for 25 hours
2. filtrationfiltered
3. customevaporated in vacuo
4. additionThe residue was treated with diluted ammonium hydroxide (10 ml)
5. extractionextracted with ethyl acetate (2×25 ml)
6. dry with materialThe organic phase was dried (MgSO4)
7. filtrationfiltered
8. customevaporated in vacuo
9. dissolutionThe residue was dissolved in diethyl ether
10. customThe precipitate was triturated with ethyl acetate
11. washwashed with diethyl ether