Sulfuric acid magnesium salt (1:1) → HCID 20330260, compound

Participants

Reaction Steps

A solution of 5.3 g of the ethyl ester from Step A in 200 ml of ether was added dropwise over about 30 minutes to a stirred mixture of 0.53 g of LiAlH4 and 50 ml of ether. After the addition was complete the mixture was stirred 1 hour at ambient temperature, warmed to reflux and allowed to cool spontaneously to ambient temperature. With vigorous stirring a saturated aqueous solution of ammonium chloride was added slowly until a granular precipitate and a clear ether phase formed. Anhydrous magnesium sulfate was added. After stirring a short time the mixture was filtered and the filtrate was concentrated to dryness to give 2.28 g of 1-methyl-4-(10,11-dihydro-3-hydroxymethyl-5H-dibenzo[a,d]-cyclohepten-5-ylidene)piperidine, m.p. 178°-181° C. after recrystallization from acetonitrile.

Provenance & Evidence