2-Methyl-2-butene → HCID 178441931, compound

Participants

Reaction Steps

A solution of the product of Example 6 (0.3 g) and 2-methyl-but-2-ene (2M in THF; 4 ml) in a mixture of THF (14 ml) and t-butanol (14 ml) was treated with a solution of sodium chlorite (80% tech. 0.55 g), and sodium dihydrogenorthophosphate (0.65 g) in water (10 ml). The mixture was stirred at ambient temperature for 2 h. The solvent was removed in vacuo and the aqueous residue acidified (pH 4.5) with hydrochloric acid (2M). The product was extracted with a mixture of dichloromethane:ethyl acetate (1:1; 25 ml) and the organic extract dried and evaporated in vacuo. The residue was crystallized from methyl acetate/hexane to give the title compound as a white solid (0.2 g), m.p. 216°-220°.

Provenance & Evidence