Galaxolide → Benzopyran

Participants

Reaction Conditions

Reaction Steps

750 grams of the liquid phase benzopyran mixture was prepared according to Example 15 of U.S. Pat. No. 3,360,530, the specification of which is herein incorporated by reference, containing 78% by weight of 1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethyl-cyclopenta[G]-2-benzopyran and 500 grams of hexane were admixed and cooled to a temperature of −30° C. with stirring. Stirring continued for a period of 1 hour at which point in time solid particles began to precipitate. The mixture was stirred for an additional 3 hours while slowly increasing the temperature of the benzopyran-solvent mixture to 0° C. The white solids were filtered at 0° C., resulting in the isolation of 240 grams of a mixture containing the following substances in the weight percentage stated:

Provenance & Evidence