反应详情

A solution of methyl 3-(1-(3-fluoro-4-(5-(1-phenylcyclopropyl)thiazolo[5,4-b]pyridine-2-yl)phenyl)cyclopropylamino)propanoate (0.031 g, 0.064 mmol) in tetrahydrofuran (0.2 mL) and methanol (0.1 mL) was added 1 M lithium hydroxide solution (0.19 mL, 0.19 mmol) and stirred at room temperature for 3 hours. The reaction mixture was concentrated in vacuo and the resulting slurry was diluted with water and neutralized (to pH=˜7) with aqueous 1 N HCl solution. The aqueous suspension was extracted with 15% MeOH/CHCl3; the organic extracts were combined, dried (K2CO3), filtered, and concentrated in vacuo. Purification via reverse phase prep. HPLC afforded the title compound as an off-white amorphous solid. MS (ESI) m/z: Calculated: 473.2; Observed: 474.1 (M++1).

1. concentrationThe reaction mixture was concentrated in vacuo
2. additionthe resulting slurry was diluted with water and neutralized (to pH=˜7) with aqueous 1 N HCl solution
3. extractionThe aqueous suspension was extracted with 15% MeOH/CHCl3
4. dry with materialdried (K2CO3)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customPurification via reverse phase prep