反应详情

To compound 23 (as per Example S above) (17 mg, 0.04 mmol) in a mixture of dry DMF (2 mL), CH2Cl2 (0.5 mL) and MeOH (0.2 mL) was added azetidine hydrochloride (16 mg, 0.17 mmol) and NaOAc (14 mg, 0.17 mnnol) under Ar(g). After 5 minutes NaBH(OAc)3 (27 m0, 0.13 mmol) and NaBH3CN (5.4 mg, 0.09 mmol) were added and the reaction mixture was stirred for 16 h. EtOAc (45 mL) was added along with 50% saturated brine (5 mL); the layers were separated, extracted with EtOAc (3×10 mL), dried (MgSO4) and concentrated in vacuo. Purification by flash column chromatography on silica (eluant 2-8% MeOH/CH2Cl2) furnished U (5.4 mg, 0.012 mmol, 28%) as an off-white solid.

1. customthe layers were separated
2. extractionextracted with EtOAc (3×10 mL)
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. customPurification by flash column chromatography on silica (eluant 2-8% MeOH/CH2Cl2)
6. customfurnished U (5.4 mg, 0.012 mmol, 28%) as an off-white solid