Phosphorus sulfide (P2S5) → HCID 54221762, compound

Participants

Reaction Conditions

Reaction Steps

1-(3,4-Dimethoxy-5-nitrophenyl)-4-(3,4,5-trimethoxyphenyl)-1,4-butanediol (4.61 g, 10.55 mmole) and 6.57 g of P4S10 were suspended in 60 mL of pyridine and heated at 90° C. for 16 hours. The solvent was removed by distillation in vacuo. The residue was acidified with 10% HCl and extracted with dichloromethane. The organic layer was washed with 10% HCl, water and saturated aqueous sodium chloride, dried over MgSO4, filtered and evaporated to give a gummy residue that was purified by flash chromatography using 3:1 hexane/ethyl acetate as the solvent (335.6 mg, 7.3%). 1H NMR (CDCl3): 2.08 (m, 2H); 2.60 (m, 2H); 3.82 (s, 3H); 3.90 (s, 6H); 3.95 (s, 3H); 3.98 (s, 6H); 4.81 (m, 2H); 6.70 (s, 2H); 7.22 (d, 1H); 7.44 (d, 1H).

Provenance & Evidence