Reaction #3078560
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04075198
Conditions: temp:75.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: 90 Parts of an aqueous solution of technical sodium hydrosulfide (35 percent NaHS, 10 percent Na2S2O3) were added to a mixture of 45.2 parts of 2,2'-dimethylazoxybenzene in 150 parts methanol at 70° C to 75° C. Subsequently, the reaction mixture was refluxed at 75° C for 4 hours with pH kept between 9 and 9.4. Thereafter, the reaction mixture was cooled down to 0° C to 5° C, and the resulting precipitate filtered off and washed with water until alkali-free. The press-cake was dried below 70° C. There were obtained 35.6 parts of 2,2'-dimethylhydrazobenzene of a melting point of 162° C to 164° C, this representing a yield of 84 percent of the theory, of acceptable purity. Thereafter, the reaction mixture was cooled down to 0° C to 5° C the resulting precipitate filtered off washed with water until alkali-free The press-cake was dried below 70° C
Source ID: ord-38251b83e2ef42499fd0f60778992634