Water → HCID 54410579, compound

Participants

Reaction Conditions

Reaction Steps

A suspension of sodium hydride (from 1.68 gms of petrol-washed 80% oil dispersion) in dimethylsulphoxide (40 mls) was stirred at 60° C. for 11/2 hours under a nitrogen atmosphere. The solution was cooled to 20° C., diluted with dry tetrahydrofuran (40 ml) and cooled to -5° C. A slurry of trimethylsulphonium iodide (11.42 gms) in dimethyl sulphoxide (30 mls) was added followed, after 10 minutes stirring, by a solution of the product of Stage 1 (4.9 g) in Tetrahydrofuran (30 mls). The mixture was stirred for 2 hours at -5° C., stood overnight at 20° C., and poured into water and extracted with petrol (30°-40° C.). The extracts were washed with brine, dried and evaporated to give 4.67 gms of yellow product. Gas chromatography showed 75% of a major component. The product was used without further purification.

Provenance & Evidence