反应详情

A solution of 4-oxo-1-phenyl-1,3,7-triaza-spiro[4.5]decane-7-carboxylic acid tert-butyl ester (130 mg, 0.45 mmol) in dry THF (3 ml) under nitrogen was cooled to −78° C. and treated with 1M LHMDS in THF (0.55 ml, 0.55 mol). The reaction was allowed to warm to RT for 30 mins before cooling back to −78° C. and adding 2M MeI in THF solution (0.45 ml, 0.9 mmol). The reaction was left to warm to RT overnight. The reaction mixture was diluted with EtOAc (10 ml) and washed with brine (20 ml). The aqueous phase was extracted with EtOAc (10 ml). Organics portions were combined, dried (MgSO4) and concentrated in vacuo. Purification of the crude product by chromatography on silica eluting with 0-50% EtOAc in iso-hexane afforded the title compound.

1. temperaturebefore cooling back to −78° C.
2. waitThe reaction was left
3. temperatureto warm to RT overnight
4. washwashed with brine (20 ml)
5. extractionThe aqueous phase was extracted with EtOAc (10 ml)
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo
8. customPurification of the crude product by chromatography on silica eluting with 0-50% EtOAc in iso-hexane