反应详情

To a solution of furo[2,3-b]pyridine-3(2H)-one (78.3 mmol) [J. Heterocyclic Chem., 23, 1465 (1986)] in 500 mL EtOH were added O-methyl-hydroxylamine (157 mmol) and NaOAc (157 mmol). After heating to reflux for 2 h the reaction mixture was concentrated in vacuo to half of its volume. Water and DCM were added and the aqueous phase was extracted 3 times with DCM. The combined organic layers were dried over MgSO4 and concentrated in vacuo. Purification by CC using Hept/EtOAc (5/1 to 1/1) gives the desired product as yellow oil;

1. temperatureAfter heating
2. temperatureto reflux for 2 h the reaction mixture
3. concentrationwas concentrated in vacuo to half of its volume
4. additionWater and DCM were added
5. extractionthe aqueous phase was extracted 3 times with DCM
6. dry with materialThe combined organic layers were dried over MgSO4
7. concentrationconcentrated in vacuo
8. customPurification by CC