Reaktion #1798211
ord-2232855a4486400383432d0a3153db46
Reaktionsgleichung
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Einengenconcentrated to dryness
- 2Extraktionextracted with EtOAc
- 3ExtraktionThe organic extract
- 4Sonstigewas collected
- 5Trocknendried over anhydrous Na2SO4
- 6Einengenconcentrated under reduced pressure
Vorschrift
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).