反应详情

To a solution of hydrazine hydrate (2.7 mL, 48.6 mmol) in EtOH (80 mL) was added ethyl 2,2,2-trifluoroacetate (6.3 mL, 48.6 mmol). The reaction was aged at room temperature for 90 minutes and concentrated in vacuo. To the crude residue was added EtOH (50 mL) and formamidine acetate (5.1 g, 48.6 mmol) and the reaction was warmed to reflux for 3 h. The reaction was cooled, concentrated in vacuo, and taken up in EtOAc and washed with sat. aq. NaHCO3 (2×). The organic layer was dried (MgSO4) and concentrated to give a pale yellow oil which was used without further purification. 1H NMR (CDCl3, 400 MHz) δ 13.6 (br s, 1H), 8.5 (s, 1H).

1. concentrationconcentrated in vacuo
2. temperaturethe reaction was warmed
3. temperatureto reflux for 3 h
4. temperatureThe reaction was cooled
5. concentrationconcentrated in vacuo
6. washwashed with sat. aq. NaHCO3 (2×)
7. dry with materialThe organic layer was dried (MgSO4)
8. concentrationconcentrated
9. customto give a pale yellow oil which
10. customwas used without further purification