Methane → HCID 18801070, compound

Participants

Reaction Steps

The product from Example 6 (3.0 g) was dissolved in dimethylsulphoxide and Pd(dba)2 (200 mg) was added. The mixture was treated with H2 at atmospheric pressure until gas uptake ceased. On completion, the reaction was added to water (500 ml) and extracted with ethyl acetate (2×400 ml). The combined organic extracts were washed with water (2×300 ml) and then dried on MgSO4, and filtered. Removal of the solvent in vacuo gave a yellow oil which was dissolved in diethyl ether, treated with charcoal, then filtered through. Hyflo. Removal of the solvent from the filtrate gave the crude title product. Precipitation from ethyl acetate/40-60° petroleum ether afforded the title product as a white solid; mp 150-151° C.

Provenance & Evidence