Phosphorus oxychloride → HCID 54161239, compound

Participants

Reaction Conditions

Reaction Steps

4-(2,5-dimethyl-4-methoxyphenyl)-2-methyl-3-buten-2-ol (18 g, 0.08M) in 25 ml of N,N-dimethylformamide (DMF) was added dropwise at 0° C. (ice bath) to the Vilsmeier reagent prepared from 15.4 g of phosphorus oxychloride and 15 ml of DMF. The resulting mixture was heated slowly to 80° C. and was stirred at this temperature for 4 hrs. The content of reaction flask was poured into 250 ml of ice-water mixture and sodium acetate (80 g) was added slowly in portions. The product was then extracted into ether. After work-up, the residue was purified by a silica gel dry column (15% ethyl acetate in hexane) to give 12 g of pure material as yellow powder, m.p. 90°-92° C. MS(CI): 231(m+ +1).

Provenance & Evidence