Methanol → HCID 136487410, compound

Participants

Reaction Steps

A mixture of 15 g (0.048 mole) of the compound of Example V, 1 tsp. of 5% Pd/C, 50% H2O, and 135 ml of methanol was shaken under hydrogen pressure with the theoretical amount of H2 being absorbed. The catalyst was removed by filtration and the solvent removed on the Calab evaporator to give a residual solid. The solid was refluxed in 750 ml of ethyl acetate, cooled in an ice bath and the insoluble material removed by filtration. The filtrate was reduced to 300 ml volume on the Calab evaporator and then diluted with hexane. The resulting solid was filtered and air dried to yield 5.4 g (46%). An analytical sample was prepared by dissolving a sample in refluxing ethyl acetate and adding hexane to the cloud point. This procedure was repeated three times, m.p. 157°-158°.

Provenance & Evidence