Ethyl trifluoroacetate → HCID 178506277, Verbindung

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

ORD-Eintrag

ord-5350c163ff2a4fdd9337e4ac319110f4

Quelldatensatz

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08530480B2