反应详情

To a solution of 22 (3.23 g, 8.33 mmol) and NiCl2.6H2O (3.96 g, 16.66 mmol) in MeOH/THF (100/100 mL) was added NaBH4 (1.24 g, 33.32 mmol). The reaction mixture was stirred for 1 hr, concentrated to dryness and the resultant solid was dissolved in 10% HCl. The aqueous solution was then made basic with concentrated NH4OH solution and extracted with EtOAc. The organic phase was collected, dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford 23 as a black solid (2.72 g, 91% yield). MS (m/z): 358.2 (M+H).

1. concentrationconcentrated to dryness
2. dissolutionthe resultant solid was dissolved in 10% HCl
3. extractionextracted with EtOAc
4. customThe organic phase was collected
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure