反应详情

Following the procedure described in Helvetica Chimica Acta (1952), 35, 478-85, 5.00 g (26.37 mmmol) of 3-nitrophenylhydrazine hydrochloride suspended in 46 ml of 55% aqueous AcOH were dissolved by careful heating and treated (without further heating) with 4.13 ml (26.37 mmol) of ethyl diacetoacetate. The reaction was immediately cooled and kept 20 h at 0° C. The precipitate was diluted with 28 ml of water and after 6 h filtered and washed with 2×5 ml of water to give after drying under reduced pressure 4.66 g (61%) of the title compound as a light yellow solid. MS: 289.9 (MH+).

1. dissolutionwere dissolved
2. temperatureby careful heating
3. additiontreated
4. temperatureThe reaction was immediately cooled
5. filtrationfiltered
6. washwashed with 2×5 ml of water
7. customto give
8. dry with materialafter drying under reduced pressure 4.66 g (61%) of the title compound as a light yellow solid