Potassium Carbonate → 6-Chloro-5-methylpyridin-3-ol

HRID 930486

反応式

HRID 930486 の反応式
C(=O)([O-])[O-].[K+].[K+].C([O:10][C:11]1[CH:12]=[N:13][C:14]([Cl:18])=[C:15]([CH3:17])[CH:16]=1)(=O)C>CO>[Cl:18][C:14]1[N:13]=[CH:12][C:11]([OH:10])=[CH:16][C:15]=1[CH3:17]

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 218288696-Chloro-5-methylpyridin-3-yl acetate

生成物 1

HCID 128520156-Chloro-5-methylpyridin-3-ol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Potassium carbonate (1.10 g, 0.0081 mol) was added to a stirred solution of 6-chloro-5-methylpyridine-3-yl acetate (750 mg, 0.004 mol) in MeOH (15 mL) at ambient temperature. The reaction mixture was stirred for 1 h at ambient temperature. The reaction mixture was concentrated under reduced pressure and the residue was diluted with minimum amounts of water and neutralized with 1N HCl (15 mL). After neutralization, the solution was extracted with ethyl acetate (2×100 mL). The combined organic layers were washed with brine, dried over anhydrous sodium sulfate and concentrated to give 6-chloro-5-methylpyridine-3-ol as an off white solid (500 mg, 89%). MS m/z=143.01 [M+H]+.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionthe residue was diluted with minimum amounts of water and neutralized with 1N HCl (15 mL)
  3. extractionAfter neutralization, the solution was extracted with ethyl acetate (2×100 mL)
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-11b1e41e244941babda06339b629afd3
出典データセット
uspto-grants-2016_03
特許番号
US09296734B2

関連ノート

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