反应详情

In a 50 mL round bottom flask, 4-{4-[3-((R)-2-methyl-pyrrolidin-1-yl)-propoxy]-phenyl}-4-oxo-2-pyridin-2-yl-butyric acid ethyl ester (950 mg, 1.84 mmol), and hydrazine monohydrate (204 μL, 4.2 mmol), in acetic acid (20 mL) was heated to reflux 14 h. The reaction was cooled and the solvent concentrated under vacuum. The slurry was partitioned between methylene chloride and NaHCO3 sol., extracted three times, and then dried over MgSO4. Purification with silica gel chromatography eluting with methylene chloride/methanol (95:5) produced 250 mg (33%). Ethereal HCl was added to a methanol solution to produce crystals. Mp 231-233° C. MS m/z 393 (M+H).

1. temperatureto reflux 14 h
2. temperatureThe reaction was cooled
3. concentrationthe solvent concentrated under vacuum
4. customThe slurry was partitioned between methylene chloride and NaHCO3 sol.
5. extractionextracted three times
6. dry with materialdried over MgSO4
7. customPurification with silica gel chromatography
8. washeluting with methylene chloride/methanol (95:5)
9. customproduced 250 mg (33%)
10. customto produce crystals