3,6-dimethylbenzene-1,2-diamine

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 2,3-diamino-p-xylene (5.1 g), formic acid (88%, 200 mL) and 12N HCl (20 mL) is heated to reflux for 3 hours. The resulting mixture is cooled to room temperature and rotary evaporated. The residue is diluted with water (100 mL), then basified with ammonium hydroxide (28-30%). The suspension is extracted with ethyl acetate (3×100 mL). The combined extracts are dried over MgSO4 and rotary evaporated to afford 4,7-dimethylbenzimidazole as a yellow solid. is heated to reflux for 3 hours The suspension is extracted with ethyl acetate (3×100 mL) The combined extracts are dried over MgSO4 rotary evaporated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 2,3-diamino-p-xylene (5.1 g), formic acid (88%, 200 mL) and 12N HCl (20 mL) is heated to reflux for 3 hours. The resulting mixture is cooled to room temperature and rotary evaporated. The residue is diluted with water (100 mL), then basified with ammonium hydroxide (28-30%). The suspension is extracted with ethyl acetate (3×100 mL). The combined extracts are dried over MgSO4 and rotary evaporated to afford 4,7-dimethylbenzimidazole as a yellow solid. is heated to reflux for 3 hours The suspension is extracted with ethyl acetate (3×100 mL) The combined extracts are dried over MgSO4 rotary evaporated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 2,3-diamino-p-xylene (5.1 g), formic acid (88%, 200 mL) and 12N HCl (20 mL) is heated to reflux for 3 hours. The resulting mixture is cooled to room temperature and rotary evaporated. The residue is diluted with water (100 mL), then basified with ammonium hydroxide (28-30%). The suspension is extracted with ethyl acetate (3×100 mL). The combined extracts are dried over MgSO4 and rotary evaporated to afford 4,7-dimethylbenzimidazole as a yellow solid. is heated to reflux for 3 hours The suspension is extracted with ethyl acetate (3×100 mL) The combined extracts are dried over MgSO4 rotary evaporated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of p-xylenediamine (2.0 g) in dichloromethane (200 ml) maintained below 10° C. was added N,N-diisopropylamine (2.52 ml) followed by the dropwise addition of acetylchloride (1.15 g). The mixture was allowed to attain room temperature and stirred overnight. Water (120 ml) was added and the suspension filtered. The filtered solid was washed with dichloromethane (2×100 ml) and water (100 ml). All filtrates were combined and the organic layer separated. The organic layer was washed with water, dried (MgSO4) and evaporated to give the title product as a solid, m.p. 133-5° C. to attain room temperature the suspension filtered The filtered solid was washed with dichloromethane (2×100 ml) and water (100 ml) the organic layer separated The organic layer was washed with water dried (MgSO4) evaporated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 5.1 g of 2,3-diamino-p-xylene, 200 mL of 88% formic acid and 20 mL of 12N hydrochloric acid is heated to reflux for 3 hours. The resulting mixture is cooled to room temperature and rotary evaporated. The residue is diluted with 100 mL of water, then basified with ammonium hydroxide (28-30%). The suspension is extracted with ethyl acetate (3×100 mL). The combined extracts are dried over magnesium sulfate and rotary evaporated to afford 4,7-dimethylbenzimidazole as a yellow solid. is heated to reflux for 3 hours The suspension is extracted with ethyl acetate (3×100 mL) The combined extracts are dried over magnesium sulfate rotary evaporated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 2,3-diamino-p-xylene (5.1 g), formic acid (88%, 200 mL) and 12N HCl (20 mL) is heated to reflux for 3 hours. The resulting mixture is cooled to room temperature and rotary evaporated. The residue is diluted with water (100 mL), then basified with ammonium hydroxide (28-30%). The suspension is extracted with ethyl acetate (3×100 mL). The combined extracts are dried over MgSO4 and rotary evaporated to afford 4,7-dimethylbenzimidazole as a yellow solid. is heated to reflux for 3 hours The suspension is extracted with ethyl acetate (3×100 mL) The combined extracts are dried over MgSO4 rotary evaporated