3-Fluorobenzoylacetonitrile synthesis
- Product Name:3-Fluorobenzoylacetonitrile
- CAS Number:21667-61-8
- Molecular formula:C9H6FNO
- Molecular Weight:163.15
Yield: 72%
Reaction Conditions:
Stage #1:methyl 3-fluorobenzoate;acetonitrile with sodium hydride in toluene at 90; for 18 h;
Stage #2: with hydrogenchloride;water; pH=5 - 6
Steps:
17.a
a) 3-(3-Fluoro-phenyl)-3-oxo-propriomlrileThe product was prepared according to a modification of general route Al . To a solution of methyl-3-fluorobenzoate (3 g, 18 mmol) in dry toluene (25 niL) under N2, NaH (50-60% dispersion in mineral oil, 1.44 g, 36 mmol) was carefully added.The mixture was heated at 9O0C and then dry CH3CN was added dropwise (4.45 niL, 85.2 mmol). The reaction was heated for 18 hours and the product precipitated from the reaction mixture as its sodium salt. The reaction was allowed to cool down to room temperature and the solid formed was filtered, then redissolved in water, and the solution was acidified with 2N HCl to pH 5-6, upon which precipitation was observed. Filtration of the solid from the aqueous solution afforded 2.12 g of the title compound (72% yield) which was used directly in the following step.
References:
SIENA BIOTECH S.P.A.;WYETH PHARMACEUTICALS WO2008/87529, 2008, A1 Location in patent:Page/Page column 111
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