3-chloro-2-methyl-3-phenylprop-2-enal

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 1.2 mol (110 mL) of POCl3 was added at 0° C. to a 2.8 mol (216 mL) of DMF (excess of DMF used as solvent). At the end of the addition, the mixture was allowed to warm to room temperature and stirred for 1 h. Then it was cooled again to 0° C. and treated with 1 mol (134 g) of propiophenone. The resulting reaction mixture was allowed to reach room temperature and stirred overnight. Then it was poured into a mixture of ice and water, added of sodium acetate and extracted with CHCl3 (3×150 mL). The organic phase was separated, washed with water until neutral pH, dried over MgSO4 and evaporated off to dryness. The residue was distilled in vacuo, b.p. 120° C./10 torr. Yield 163 g (90%). At the end of the addition Then it was cooled again to 0° C. The resulting reaction mixture to reach room temperature stirred overnight extracted with CHCl3 (3×150 mL) The organic phase was separated washed with water until neutral pH dried over MgSO4 evaporated off to dryness The residue was distilled in vacuo, b.p. 120° C./10 torr