3-Acetoxy-6-fluoro-5-methylpyridine → 6-Fluoro-5-methylpyridin-3-ol
反応式
C([O:4][C:5]1[CH:6]=[N:7][C:8]([F:12])=[C:9]([CH3:11])[CH:10]=1)(=O)C>[OH-].[Na+]>[F:12][C:8]1[C:9]([CH3:11])=[CH:10][C:5]([OH:4])=[CH:6][N:7]=1参加物
3
実験手順
The product of step 32d (3.6 g, 21.3 mmol) was dissolved in 20% aqueous NaOH (25 mL). After complete consumption of the starting material the solution was neutralized by addition of HCl. The aqueous mixture was extracted with ethyl acetate. The organic extracts were dried (MgSO4), and the solvent was evaporated. The crude product was triturated with hexane to yield 2.35 g (87%) of the title compound: MS (CI/NH3) m/z: 128 (M+H)+, 145 (M+NH4)+ ; 1H NMR (CDCl3, 300 MHz) δ: 7.61(t, J=2.2 Hz, 1H), 7.17 (m, 1 H), 2.25 (s, 3H).
後処理
- customAfter complete consumption of the starting material the solution
- additionwas neutralized by addition of HCl
- extractionThe aqueous mixture was extracted with ethyl acetate
- dry with materialThe organic extracts were dried (MgSO4)
- customthe solvent was evaporated
- customThe crude product was triturated with hexane
出典と根拠
- ORDレコード
- ord-c229255d6d3c4668a0b36798cf316587
- 出典データセット
- uspto-grants-2000_10
- 特許番号
- US06133253
反応ノート
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