Dicyclohexylcarbodiimide → HCID 21433911, compound

Participants

Reaction Steps

0.7 g. (2.33 mmoles) of 1-Hydroxy-3-(phenyl- 1-methylbutyl)-6,6,9-trimethyl-6a,7,8,10a-tetrahydrodibenzo [b,d]pyran, prepared according to the method of Example 48, 0.48 g. (2.28 mmoles) of γ-morpholinobutyric acid hydrochloride (Cruichshank and Sheehan, J. Am. Chem. Soc. 83, 2891 (1961), m.p. 180°-182° ) and 0.48 g. (2.35 mmoles) of dicyclohexylcarbodiimide (Aldrich) are combined with 35 ml. of methylene chloride and stirred at room temperature for a total of 40 hours. The insoluble by-product of dicyclohexylurea is removed using a rotary evaporator. The resulting residue is dissolved in about 20 ml. of benzene and a small amount of insoluble material is removed by filtration. The benzene is evaporated and the residue dried in vacuo to give 0.7 g. of material. Crystallization from benzene/pet ether yields the crystalline product.

Provenance & Evidence