反应详情

A solution of (3-fluoro-4-(4-hydroxypyrimidin-5-yl)pyridin-2-yl)(4-fluorophenyl)methanone (0.168 g, 0.536 mmol) and hydroxylamine hydrochloride (0.039 g, 0.563 mmol) in Pyridine (Volume: 2.68 ml) was refluxed for 1.5 hr, allowed to cool to room temperature, and then concentrated in vacuo. Solvent was evaporated. The crude material was dissolved in a minimal amount of CH2Cl2 to be chromatographed (required a few drops of MeOH). Purification of the crude material by silica gel chromatography using an ISCO machine (24 g column, 35 mL/min, 1-25% MeOH in CH2Cl2 over 19 min, tr=12 min) gave the title compound (0.123 g, 0.371 mmol, 69.2% yield) as a tan solid. ESI MS (M+H)+=329.1.

1. concentrationconcentrated in vacuo
2. customSolvent was evaporated
3. dissolutionThe crude material was dissolved in a minimal amount of CH2Cl2
4. customto be chromatographed (required a few drops of MeOH)
5. customPurification of the crude material by silica gel chromatography
6. customan ISCO machine (24 g column, 35 mL/min, 1-25% MeOH in CH2Cl2 over 19 min, tr=12 min)