反应详情

To an ice-cooled solution of potassium tert.-butylate (1.71 g, 15.2 mmol) in methanol (50 mL), hydroxylamine hydrochloride (905 mg, 13.02 mmol) is added. The suspension is stirred for 30 min before 2-dimethylamino-6-methyl-isonicotinonitrile (699 mg, 4.34 mmol) is added. The mixture is refluxed for 2 h before it is evaporated. The residue is dissolved in a small amount of water and separated by MPLC on RP-C18-silica gel to give 2-dimethylamino-N-hydroxy-6-methyl-isonicotinamidine (284 mg) as a brownish resin; LC-MS: tR=0.60 min, [M+1]+=195.42.

1. additionis added
2. additionis added
3. temperatureThe mixture is refluxed for 2 h before it
4. customis evaporated
5. dissolutionThe residue is dissolved in a small amount of water
6. customseparated by MPLC on RP-C18-silica gel