p-Toluenesulfonic acid → HCID 13557855, compound

Participants

Reaction Steps

To a stirred solution of 0.8 g of p-toluenesulfonic acid in 125 ml of methanol held at 3°-5° C. was added dropwise over 0.5 hour a solution of 15.2 g of 2,2,6-trimethyl-1-oxaspiro(2.5)oct-5-ene in 25 ml of methanol. After an additional 2 hours at 5° C. and 2 hours at 5°-20° C., the mixture was treated with 2 ml of 15% sodium hydroxide and concentrated at a water pump at below 60° C. The residue was dissolved in methylene chloride, washed, dried and Claisen-distilled to give 15.6 g of the desired product, b.p. 70° C. (0.2 mm).

Provenance & Evidence