反应详情

A mixture of the product of step (ii) (0.55 g) and lithium hydroxide monohydrate (0.46 g) in methanol (10 ml) and water (10 ml) was stirred at room temperature for 3 hours. The solution was concentrated under reduced pressure to 10 ml and partitioned between 2M hydrochloric acid and ethyl acetate. The organic phase was dried (MgSO4) and the solvent evaporated under reduced pressure. Purification was by reverse phase chromatography eluting with 50% methanol in 0.1% aqueous ammonium acetate followed by lyophilisation.

1. concentrationThe solution was concentrated under reduced pressure to 10 ml
2. custompartitioned between 2M hydrochloric acid and ethyl acetate
3. dry with materialThe organic phase was dried (MgSO4)
4. customthe solvent evaporated under reduced pressure
5. customPurification
6. washeluting with 50% methanol in 0.1% aqueous ammonium acetate