反应详情

To a solution of (S)-3-methyl-2-((R)-1-(pyridin-2-yl)propylamino)butan-1-ol (step 2, crude product) (40.8 mmol) in MeOH (250 ml) was added methylamine (60 ml of a 40% aqueous solution) followed by a solution of periodic acid (37.2 g, 163 mmol) in water (70 ml). The mixture was stirred at RT overnight and the resulting white solid precipitate was filtered off. The filtrate was concentrated in vacuo to remove the MeOH. The residual aqueous layer was then extracted with EtOAc. The combined organic layers were dried (MgSO4), filtered and concentrated in vacuo Purification of the crude product by chromatography on silica eluting with a 0-20% MeOH/DCM gradient affords the title product; [M+H}+137.

1. filtrationthe resulting white solid precipitate was filtered off
2. concentrationThe filtrate was concentrated in vacuo
3. customto remove the MeOH
4. extractionThe residual aqueous layer was then extracted with EtOAc
5. dry with materialThe combined organic layers were dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo Purification of the crude product by chromatography on silica eluting with a 0-20% MeOH/DCM gradient