3-Methyl-3-buten-1-ol → HCID 20300337, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of p-TSA (20 g, 0.105 mol) and toluene (2 L) was heated to 115° C. To this mixture were added 3,3,5-trimethyl cyclohexanone (1.4 kg, 10 mols) and isoprenol (946 g, 11 mols) and heated further for 3-6 h. Water was removed from the reaction azeotropically. The reaction mixture was then cooled to room temperature. The organic phase was washed with a 5% Na2CO3 solution, washed with water dried and concentrated and distilled further to provide to 4,8,8,10-tetramethyl-1-oxaspiro [5.5] undec-3-ene (1.45 kg) having a purity of 94% (sum of the isomers) for a total yield of 55%.

Provenance & Evidence