Hydrochloric Acid → HCID 11356889, compound

Participants

Reaction Steps

Lithium amide (12.4 g, 498 mmol) was dissolved in 130 mL of methyl t-butyl ether (MTBE), and a solution of 32.4 g (253 mmol) of octan-2-one in MTBE (67 mL) was dropped under a nitrogen atmosphere at 35° C. and the mixture was stirred for 1 hour. Then, into this was dropped a solution of 80.0 g (506 mmol) of ethyl pentanoate in MTBE (67 mL), and the mixture was stirred at 35° C. for 4.5 hours. After cooling, the resultant mixed liquid was added into concentrated hydrochloric acid containing ice added, and the oil phase was extracted and died over sodium sulfate, then, concentrated. For purification of the resultant concentrate, a copper acetate aqueous solution was added to cause crystallization of a copper complex of the concentrate, which was dissolved in MTBE and mixed with a sulfuric acid aqueous solution and the mixture was returned to the concentrate, and the oil phase was extracted and dried over sodium sulfate and concentrated, to obtain 36.3 g (151 mmol) of pentadecane-7,9-dione.

Provenance & Evidence