Reaktion #73463

Reaktionsgleichung

1-cyano-1-(3-fluorophenyl)-3-methoxycarbonylcyclohexan-4-one

1-Cyano-1-(3-fluorophenyl)-3-methoxycarbonylcyclohexan-4-one

water

→

desired material

Ausbeute 69.7%

1-Cyano-1-(3-fluorophenyl)cyclohexan-4-one

Ausbeute 69.7%

Lösungsmittel

DMSO

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   workup.STIRRINGby stirring at room temperature overnight
3. 3
   SonstigeThe reaction mixture was evaporated
4. 4
   Sonstigepurified by chromatography on silica gel
5. 5
   WaschenElution with ethyl acetate/heptane (5%:95% to 30%:70%)

Vorschrift

A mixture of 1-cyano-1-(3-fluorophenyl)-3-methoxycarbonylcyclohexan-4-one (57, 51 g, 185 mmol), water (54.8 mL) and DMSO (840 mL) was heated and stirred at 150° C. for 3 hours, followed by stirring at room temperature overnight. The reaction mixture was evaporated and purified by chromatography on silica gel. Elution with ethyl acetate/heptane (5%:95% to 30%:70%) gave 28 g of desired material as a solid product. Rt=3.89 min (Method 3). Detected mass: 218.2 (M+H+).

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