3-Acetoxy-6-fluoro-5-methylpyridine → 6-Fluoro-5-methylpyridin-3-ol

HRID 2185736

反応式

HRID 2185736 の反応式
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

反応物 1

HCID 224516053-Acetoxy-6-fluoro-5-methylpyridine

生成物 1

HCID 229897166-Fluoro-5-methylpyridin-3-ol収率 87%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

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

  1. customAfter complete consumption of the starting material the solution
  2. additionwas neutralized by addition of HCl
  3. extractionThe aqueous mixture was extracted with ethyl acetate
  4. dry with materialThe organic extracts were dried (MgSO4)
  5. customthe solvent was evaporated
  6. customThe crude product was triturated with hexane

出典と根拠

ORDレコード
ord-b0ac13076dc644fdbf550c3adab0f66b
出典データセット
uspto-grants-2002_06
特許番号
US06403575B1

関連ノート

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