Dimethylformamide → HCID 53832421, compound

Participants

Reaction Steps

POCl3 (185 g) was added to 185 g of DMF at such a rate as to maintain the temperature below 25° by ice bath cooling. After stirring for 30 min, 4-methoxypropiophenone (82.1 g) was added dropwise to the mixture at 60°-65°. The reaction was maintained at 80°-90° for 8 hrs. Toluene (174 g) was added and 1-liter of a saturated sodium acetate solution was added so that a temperature of 65° was maintained by ice bath cooling. After heating at 70°-80° for 2 hrs. the organic phase was separated and washed with 300 ml of 5% NaHCO3. Distillation yielded 90 g (86%) of the desired product, bp 130° (1.0 mm).

Provenance & Evidence