反应详情

温度

50 °C

To a solution of 3-(methoxyimino)-2,3-dihydrofuro[2,3-c]pyridine 6-oxide (5.35 mmol) in 30 mL DCM were added 2.9 mL phosphoryl chloride at 0° C. The mixture was heated to 50° C. for 7 h, concentrated in vacuo, redissolved in DCM and quenched with solid NaHCO3 and then water. The aqueous layer was extracted with DCM (2×). The combined organic layers were dried over MgSO4 and concentrated in vacuo. Purification by CC (KP-SIL™ from Biotage) using Hept/EtOAc (8/2) gives the desired product as beige solid;

1. concentrationconcentrated in vacuo
2. dissolutionredissolved in DCM
3. customquenched with solid NaHCO3
4. extractionThe aqueous layer was extracted with DCM (2×)
5. dry with materialThe combined organic layers were dried over MgSO4
6. concentrationconcentrated in vacuo
7. customPurification by CC (KP-SIL™ from Biotage)