Phosphorus oxide (P4O10) → HCID 18635748, compound

Participants

Reaction Steps

An intimate mixture of Compound E (1.24 g) and phosphorus pentoxide (0.6 g) was heated to 165°. Two further aliquots of phosporus pentoxide (0.6 g each) were added at 10 minute intervals, mixing well in, while maintaining the temperature in the range 165° to 180°. Ten minutes after the final addition the solid mass was triturated with aqueous potassium hydroxide, ethyl acetate mixture and stirred well until free of solid. Evaporation of the organic layer gave a brown oil which was chromatographed on silica gel (50 g). Elution with ethyl acetate:petrol b.pt. 60°-80° (1:1) gave an oil (0.8 g) which solidified on trituration, with petrol, b.pt. 60°-80°. The product was collected, washed with petrol and dried to give the title compound as a buff coloured solid (0.57 g) m.pt. 101°-103°, NMR τ (CDCl3) 2.74 (5H, s, Ph), 2.5-3.4 (3H, m, aromatic), 5.4-6.1 (2H, m, 3a-H, 9a-H), 6.18 (2H, s, CH2Ph), 6.5-7.4 (4H, m, 1-H2, 3-H2).

Provenance & Evidence