Under nitrogen, ketone product (0.1 mmol) and TsNHNH2 (0.2 mmol, 37.2 mg) were dissolved
in dry MeOH (2.5 mL). The mixture was stirred at 60 o
C until the ketone was completely
consumed (monitored by TLC). After completion, MeOH was evaporated under reduced
pressure. The residue was dissolved in dry EtOH (2.5 mL) without separation and NaBH4 (0.6
mmol, 22.7 mg) was added. The resulting mixture was stirred at 40 o
C for 1 h. After completion,
EtOH was evaporated under reduced pressure and the residue was purified by flash
chromatography to give the corresponding product,
Under nitrogen, ketone product (0.1 mmol) and TsNHNH2 (0.2 mmol, 37.2 mg) were dissolved
in dry MeOH (2.5 mL). The mixture was stirred at 60 o
C until the ketone was completely
consumed (monitored by TLC). After completion, MeOH was evaporated under reduced
pressure. The residue was dissolved in dry EtOH (2.5 mL) without separation and NaBH4 (0.6
mmol, 22.7 mg) was added. The resulting mixture was stirred at 40 o
C for 1 h. After completion,
EtOH was evaporated under reduced pressure and the residue was purified by flash
chromatography to give the corresponding product,
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