反应详情

At 0° C., KOtBu (1.81 g, 16.2 mmol) is carefully added to methanol (25 mL). Hydroxylamine hydrochloride (963 mg, 13.9 mmol) is then added to this solution. The suspension is stirred for 30 min before 2-ethyl-6-methyl-isonicotinonitrile (675 mg, 4.62 mmol) is added. The mixture is refluxed for 1 h, the solvent is evaporated. The residue is dissolved in water, extracted three times with EA. The org. extracts are dried over MgSO4, filtered, evaporated and dried under HV to give 2-ethyl-N-hydroxy-6-methyl-isonicotinamidine (897 mg) as a white powder, LC-MS: tR=0.31 min, [M+1]+=180.32.

1. additionis added
2. temperatureThe mixture is refluxed for 1 h
3. customthe solvent is evaporated
4. dissolutionThe residue is dissolved in water
5. extractionextracted three times with EA
6. dry with materialextracts are dried over MgSO4
7. filtrationfiltered
8. customevaporated
9. customdried under HV