反应详情

To a solution of 256 (168.4 mg, 0.478 mmol) and NiCl2×6H2O (226 mg, 0.956 mmol) in MeOH/THF (10/10 mL) NaBH4 (72 mg, 1.92 mmol) was carefully added. The reaction mixture was stirred for 10 min, concentrated to dryness and the resultant solid was suspended in 10% HCl. The aqueous solution was basified (pH˜11) with concentrated aqueous NH4OH and extracted with EtOAc. The organic extract was collected, dried over anhydrous Na2SO4 and concentrated under reduced pressure, to afford title compound 257 (134.6 mg, 87% yield) as a white solid. MS (m/z): 322.09 (M+1).

1. concentrationconcentrated to dryness
2. extractionextracted with EtOAc
3. extractionThe organic extract
4. customwas collected
5. dry with materialdried over anhydrous Na2SO4
6. concentrationconcentrated under reduced pressure