Acetic Acid → HCID 549741, compound

Participants

Reaction Steps

125 g of crude 3-bromo-2,6,6-trimethyl-1-(but-2-enoyl)-cyclohex-1-ene [prepared under letter a] were added dropwise to a mixture of 100 g (1 Mole) CrO3, 100 ml acetic acid and 100 ml of water, kept at 20°-25°. After addition of the reactants the reaction mixture was heated under stirring at 40° for 30 min., and finally diluted with 1 l of water. After neutralization of the reactin mixture by means of a 10 % aqueous solution of NaOH, the obtained mixture was submitted to a steam distillation. 3 l of the thus obtained distillate were then extracted with ether (3 × 500 ml), the organic layer was washed with water, dryed over Na2SO4 and finally concentrated under reduced pressure. There were thus obtained 68.2 g (73 %) of a semi-cristalline product, b.p. 71°-116°/o.01 Torr, which was finally cristallized in hexane to afford 51.3 g (55 %) of pure 2,6,6-trimethyl-1-(but-2-enoyl)-cyclohex-1-en-3-one, m.p. 68°-69°.

Provenance & Evidence