2,3-diaminophenol;dihydrochloride

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In a 50 ml single neck round bottom flask, under a nitrogen atmosphere, 4-methylphenoxyacetonitrile (2.79 mmol) was admixed in methanol (11 ml). The contents were stirred to achieve dissolution. To this solution were added sodium methoxide (0.164 g, 3.0 mmol). The resulting mixture was stirred for about 40 minutes. To this mixture was added 2,3-diaminophenol dihydrochloride salt (0.5 g, 2.5 mmol) and the resulting mixture was stirred for two hours at room temperature. The reaction mixture was filtered and the filtrate was added to 60 ml of water. A light brown precipitate formed and this precipitate is removed by filtration, and washed with 20 ml of water. The solid was dried in a vacuum oven overnight. dissolution The resulting mixture was stirred for about 40 minutes the resulting mixture was stirred for two hours at room temperature The reaction mixture was filtered the filtrate was added to 60 ml of water A light brown precipitate formed this precipitate is removed by filtration washed with 20 ml of water The solid was dried in a vacuum oven overnight

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In a 50 ml single neck round bottom flask, under a nitrogen atmosphere, 4-chlorophenoxyacetonitrile (0.46 g, 2.79 mmol) was admixed in methanol (11 ml). The contents were stirred to achieve dissolution. To this solution were added sodium methoxide (0.164 g, 3.0 mmol). The resulting mixture was stirred for about 40 minutes. To this mixture was added 2,3-diaminophenol dihydrochloride salt (0.5 g, 2.5 mmol) and the resulting mixture was stirred for two hours at room temperature. The reaction mixture was filtered and the filtrate was added to 60 ml of water. A light brown precipitate formed and this precipitate is removed by filtration, and washed with 20 ml of water. The solid was dried in a vacuum oven overnight. dissolution The resulting mixture was stirred for about 40 minutes the resulting mixture was stirred for two hours at room temperature The reaction mixture was filtered the filtrate was added to 60 ml of water A light brown precipitate formed this precipitate is removed by filtration washed with 20 ml of water The solid was dried in a vacuum oven overnight

Conditions: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In a 250 ml single neck round bottom flask was added 2,3-diaminophenol (10 g, 80.55 mmol) to ethanol (100 ml). This mixture was heated to 50° C. to achieve dissolution. The resulting solution is cooled to −5 to 0° C. and an excess of anhydrous hydrogen chloride gas was added to form a viscous slurry. The resulting mixture was stirred for two hours at ˜0° C., then filtered, and rinsed with chilled methanol (30 ml). The solvents were removed in vacuo and the residue was dried overnight. dissolution The resulting solution is cooled to −5 to 0° C. to form a viscous slurry filtered rinsed with chilled methanol (30 ml) The solvents were removed in vacuo the residue was dried overnight