Methane → 2-Chloro-6-methylpyridin-3-ol

HRID 1994237

反応式

HRID 1994237 の反応式
[OH:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:8])=[N:6][CH:7]=1.C.[ClH:10]>CO>[Cl:10][C:7]1[C:2]([OH:1])=[CH:3][CH:4]=[C:5]([CH3:8])[N:6]=1

参加物

5

実験手順

5-Hydroxy-2-methylpyridine (1-014-01) (27.01 g) was dissolved in conc. hydrochloric acid (200 mL) and to the reaction mixture was bubbled chlorine gass at 68 to 74° C. After the reaction mixture was stood overnight, the volatile was removed by bubbling nitrogen gas. The reaction mixture was evaporated under reduced pressure to give the crystal residue. The crystal residue was dissolved in methanol, and treated with active charcoal. After recrystallization, the desired 2-chloro-3-hyroxy-6-methylpyridine (1-014-02) (23.96 g, 67.3%) was obtained.

後処理

  1. customwas bubbled chlorine gass at 68 to 74° C
  2. customthe volatile was removed
  3. customby bubbling nitrogen gas
  4. customThe reaction mixture was evaporated under reduced pressure
  5. customto give the crystal residue
  6. customAfter recrystallization

出典と根拠

ORDレコード
ord-1a9b304651534acbb6650440df47fa5e
出典データセット
uspto-grants-2010_01
特許番号
US07652141B2

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