Galaxolide → Benzopyran

Participants

Reaction Steps

200 grams of the liquid phase benzopyran mixture was prepared according to Example 15 of U.S. Pat. No. 3,360,530 containing 78% by weight of 1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethyl-cyclopenta[G]-2-benzopyran and 100 grams of 10% aqueous ethanol were admixed and cooled to a temperature of +5° C. with stirring. Stirring continued for a period of 2 hours at which point in time solid particles began to precipitate. The mixture was stirred for an additional 3 hours at 5° C. 42 grams of white crystalline material were filtered at 5° C. The resulting composition was a solid phase benzopyran mixture containing 91 weight % of 1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethylcyclopenta[G]-2-benzopyran having a melting point of 31° C.

Provenance & Evidence