反应详情

To 2,6-dimethylisonicotinic acid (1.00 g, 6.61 mmol) in DCM (8.3 mL), CDI (1.18 g, 7.27 mmol) was added and the mixture was stirred for 45 minutes after which N,O-dimethylhydroxylamine hydrochloride (0.71 g, 7.3 mmol) was added and the mixture was stirred for 20 hours. The reaction mixture was quenched with 0.3 M aqueous solution of NaOH and partitioned between water and DCM. The aqueous layer was extracted with DCM, washed with aqueous saturated solution of NaCl, dried (MgSO4) and concentrated. The crude product was purified by flash column chromatography (silica gel, 0-100% EtOAc-DCM) to provide the title compound.

1. additionwas added
2. customThe reaction mixture was quenched with 0.3 M aqueous solution of NaOH
3. custompartitioned between water and DCM
4. extractionThe aqueous layer was extracted with DCM
5. washwashed with aqueous saturated solution of NaCl
6. dry with materialdried (MgSO4)
7. concentrationconcentrated
8. customThe crude product was purified by flash column chromatography (silica gel, 0-100% EtOAc-DCM)