Hydrochloric Acid → HCID 13020700, compound

Participants

Reaction Steps

To a solution of 4,5α-epoxy-3-methoxy-17-methyl-morphinan-6-one (1a, 30.0 g, 0.10 mole) in dioxane (500 ml) was added H2O (600 ml), Ca(OH)2 (14.0 g. 0.19 mole) and 37% w/w formaldehyde solution (140 ml, 1.86 mole). The mixture was stirred at room temperature overnight and then concentrated under reduced pressure. The residue was diluted with H2O and extracted with EtOAc. Processing in the usual manner gave a white foam which was converted to the HCl salt. Crystallization from aqueous EtOH gave 28.7 g (72%) of 2a in three crops. Recyrstallization from aqueous EtOH gave pure 2a. HCl, mp>265°. Elemental analysis was consistent with this formula.

Provenance & Evidence