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Sodium Hydroxide → 1-methyl-4-(trifluoromethyl)-1H-pyrazole-3-carboxylic acid

HRID 1192958
ノート
印刷プレビュー

反応式

HRID 1192958 の反応式
C([O:3][C:4]([C:6]1[C:10]([C:11]([F:14])([F:13])[F:12])=[CH:9][N:8]([CH3:15])[N:7]=1)=[O:5])C.[OH-].[Na+]>CO>[CH3:15][N:8]1[CH:9]=[C:10]([C:11]([F:13])([F:14])[F:12])[C:6]([C:4]([OH:5])=[O:3])=[N:7]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 57574534Ethyl 1-methyl-4-(trifluoromethyl)-1H-pyrazole-3-carboxylate

生成物 1

HCID 597395521-methyl-4-(trifluoromethyl)-1H-pyrazole-3-carboxylic acid収率 100.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

1-Methyl-4-trifluoromethyl-1H-pyrazole-3-carboxylic acid ethyl ester (20 g, 90 mmol) was dissolved in methanol (100 ml). Sodium hydroxide in methanol (1M) (95 ml, 95 mmol) was added dropwise. The mixture was stirred at room temperature for 2 hours, stored at room temperature for 16 hours and concentrated. The residue was dissolved in aqueous hydrochloric acid (2M) (55 ml) and isopropyl acetate (300 ml). The two phases were separated and the aqueous phase was extracted with more isopropyl acetate (100 ml). The combined organic extracts were dried over magnesium sulfate and concentrated. This gave the product as a white solid (17.5 g, 100% yield). M.p. 174-175° C.

後処理

  1. waitstored at room temperature for 16 hours
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in aqueous hydrochloric acid (2M) (55 ml)
  4. customThe two phases were separated
  5. extractionthe aqueous phase was extracted with more isopropyl acetate (100 ml)
  6. dry with materialThe combined organic extracts were dried over magnesium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-10bb3bd29a7f423894ada258a73bbca2
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08680290B2

反応ノート

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