Potassium Hydroxide → 3-(Trifluoromethyl)pyrazine-2-carboxylic acid

HRID 604824ノート

反応式

HRID 604824 の反応式
[F:1][C:2]([F:14])([F:13])[C:3]1[C:4]([C:9]([O:11]C)=[O:10])=[N:5][CH:6]=[CH:7][N:8]=1.[OH-].[K+]>C(O)C.O>[F:14][C:2]([F:1])([F:13])[C:3]1[C:4]([C:9]([OH:11])=[O:10])=[N:5][CH:6]=[CH:7][N:8]=1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 58542464Methyl 3-(trifluoromethyl)pyrazine-2-carboxylate

生成物 1

HCID 536308603-(Trifluoromethyl)pyrazine-2-carboxylic acid収率 63%

試薬・触媒・溶媒 1

HCID 19096565Water ethanol溶媒

実験手順

Methyl 3-trifluoromethylpyrazine-2-carboxylate (700 mg, 3.4 mmol) was dissolved in ethanol-water (1:1, 10 ml), followed by adding potassium hydroxide (300 mg) and refluxing under heating for 1 hour. The reaction solution was concentrated under reduced pressure, followed by dilution of residue with water and washing with ethyl acetate. The water layer was acidified with HCl, followed by extracting with ethyl acetate, washing with a saturated brine. The solution was dried over magnesium sulfate, and concentrated under reduced pressure to obtain 409 mg of the desired compound as crystal.

後処理

  1. temperaturerefluxing
  2. temperatureunder heating for 1 hour
  3. concentrationThe reaction solution was concentrated under reduced pressure
  4. washwashing with ethyl acetate
  5. extractionby extracting with ethyl acetate
  6. washwashing with a saturated brine
  7. dry with materialThe solution was dried over magnesium sulfate
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1ba288a353424b96977a68062f07fada
出典データセット
uspto-grants-2011_03
特許番号
US07910735B2

反応ノート

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