Acetic Acid → HCID 14940540, compound

Participants

Reaction Steps

In a 1-neck 500 ml flask topped with a reflux condenser 250 ml of acetic acid, 50 ml of conc. hydrochloric acid and 50 ml of water were mixed together. To this mixture was added 27.7 g (0.0846 mole) of 3-carboxymethyl-3methyl-1,2,3,4-tetrahydro-4-phenanthron and the reaction mixture was refluxed for 31/2 hours under nitrogen. The mixture was diluted with 300 ml water and cooled in the refrigerator overnight. Next morning offwhite solids were collected by filtration, washed with water and dried under vacuum to give 16.9 g (95.02% by weight yield) of 3-methyl-1,2,3,4-tetrahydro-4-phenanthrone as an off-white solid. M.P. 61°-63° C.; M/e 211; λmax 309 (6,970) methanol.

Provenance & Evidence