Acetic Acid → Mls000756290

Participants

Reaction Steps

A mixture of 125 g (0.6 mole) of compound III, 214 g (2.1 moles) of acetic anhydride, 1.2 ml of Raney nickel and 36 g (0.6 mole) of acetic acid was hydrogenated at 80° C and a pressure of 100 to 30 kg/sq.cm for 5 h. After cooling, the catalyst was filtered, and the filtrate was concentrated by normal pressure until 135 ml of distillate were collected. Then 150 ml of 6N sulphuric acid were added to the residue. The reaction was very exothermic. The solution was refluxed with active carbon for 15 min and filtered. The filtrate was mixed with 1.2 kg of ice and exactly neutralized with 2N sodium hydroxide. The precipitate was washed with water and dried at 100° C. Melting point: 251° C. Yield: 88% (108 g).

Provenance & Evidence