Reaktion #798691

Reaktionsgleichung

P2O5

2,2,2-trifluoroethane-1,1-diol

CH3NO2

Na2CO3

→

3,3,3-Trifluoro-1-nitroprop-1-ene

Ausbeute 10.0%

Lösungsmittel

Water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe mixture was extracted with diethyl ether (3×30 mL)
2. 2
   Trocknendried over Na2SO4
3. 3
   EinengenAfter concentrating the
4. 4
   workup.ADDITIONwas added to the residue oil, which
5. 5
   workup.DISTILLATIONwas distilled at atmospheric pressure
6. 6
   Sonstigeto give a green-yellow oil (4 g, 50% purity, 10% yield)

Vorschrift

A mixture of 2,2,2-trifluoroethane-1,1-diol (75% aq solution, 20 g, 0.13 mol), CH3NO2 (24 g, 0.39 mol) and Na2CO3 (0.85 g, 8 mmol) was stirred overnight at RT. Water (50 mL) was added and the mixture was extracted with diethyl ether (3×30 mL) and dried over Na2SO4. After concentrating the organic extract at low temperature and under reduced pressure, P2O5 (20.0 g, 0.14 mol) was added to the residue oil, which was distilled at atmospheric pressure to give a green-yellow oil (4 g, 50% purity, 10% yield). Boiling point 85-90° C.; 1H NMR (400 MHz, CDCl3) δ ppm 7.09-7.17 (m, 1H), 7.50 (dd, J=2.0 Hz, 12.0 Hz, 1H).

Quelle