Acetic acid, 2-(4,4-difluorocyclohexylidene)-, ethyl ester synthesis
- Product Name:Acetic acid, 2-(4,4-difluorocyclohexylidene)-, ethyl ester
- CAS Number:1283719-20-9
- Molecular formula:C10H14F2O2
- Molecular Weight:204.21
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Yield:1283719-20-9 97%
Reaction Conditions:
in tetrahydrofuran at 65;Inert atmosphere;
Steps:
3
Compound 3.1. Ethyl 2-(4,4-difluorocyclohexylidene)acetate. A solution of 4,4- difluorocyclohexan-l-one (1.0 g, 7.46 mmol, 1.00 equiv) and (carbethoxymethylene)triphenylphosphorane (3.9 g, 24.05 mmol, 1.50 equiv) in THF (20 mL) was stirred under argon overnight at 65 °C. After cooling to ambient temperature, the mixture was concentrated under reduced pressure and the crude residue was purified using flash column chromatography (silica gel, EtOAc / petroleum ether (1 : 10)) to yield 1.5 g (97%) of a colorless oil. 1H-NMR (400 MHz, CDC13): δ ppm 5.75 (s, 1H), 4.18 (m, 2H), 3.06 (t, J = 6.8 Hz, 2H), 2.34 (t, J = 6.8 Hz, 2H), 2.11 - 1.99 (m, 4H), 1.33 - 1.26 (m, 3H).
References:
WO2014/205234,2014,A1 Location in patent:Paragraph 0076
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22515-18-0
254 suppliers
$5.00/100mg
1283719-20-9
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