2-(4-FLUOROBENZOYL)-3-(DIMETHYLAMINO) ACRYLONITRILE synthesis

Yield:-

Reaction Conditions:

at 20; for 0.25 h;

Steps:

2.16.i Step i)
[00476] To 3-(4-Fluoro-phenyl)-3-oxo-propionitrile (3 g, 18.3 mmol, 1 eq.) is added N,N- Dimethylformamide dimethyl acetal (7.32 mL, 55.163 mmol, 3 eq.). The reaction mixture is stirred at r.t. for 15 min. The reaction mixture is diluted with water, and the solid is filtered off, washed with water and dried in vacuo. The crude is purified by cake of silica gel (elution with DCM/MeOH : 100/3) to afford the expected product. [00477] LC-MS : MW (calcd) : 218 ; m/z MW (obsd) : 219 ( M+H) Step ii)

References:

GALAPAGOS NV;DESROY, Nicolas;HECKMANN, Bertrand;BRYS, Reginald Christophe Xavier;JONCOUR, Agnès Marie;PEIXOTO, Christophe;BOCK, Xavier Marie;HOUSSEMAN, Christopher Gaëtan WO2014/202458, 2014, A1 Location in patent:Paragraph 00476; 00477