反应详情

To a solution of 4-oxo-1-phenyl-1,3,7-triaza-spiro[4.5]dec-2-ene-7-carboxylic acid tert-butyl ester (130 mg, 0.39 mmol) in methanol (3 ml) was added sodium borohydride (22 mg, 0.59 mmol). The reaction mixture was stirred at RT for 1 hour. The reaction mixture was concentrated in vacuo. The residue was dissolved with EtOAc (5 ml) and washed with a saturated solution of sodium bicarbonate (10 ml). The aqueous phase was extracted with further EtOAc (5 ml). The organics portions were combined, dried (MgSO4) and concentrated in vacuo to afford an oil. Purification of the crude product by chromatography on silica eluting with 0-50% EtOAc in iso-hexane afforded the title compound.

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutionThe residue was dissolved with EtOAc (5 ml)
3. washwashed with a saturated solution of sodium bicarbonate (10 ml)
4. extractionThe aqueous phase was extracted with further EtOAc (5 ml)
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. customto afford an oil
8. customPurification of the crude product by chromatography on silica eluting with 0-50% EtOAc in iso-hexane