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Lithium Hydroxide → HCID 58972822、化合物

HRID 12915
ノート
印刷プレビュー

反応式

HRID 12915 の反応式
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([C:15]([CH3:19])([CH3:18])[CH2:16][OH:17])[C:10]=1[C:11]([F:14])([F:13])[F:12])=[O:5])C.[Li+].[OH-]>CO.O>[OH:17][CH2:16][C:15]([N:9]1[C:10]([C:11]([F:12])([F:13])[F:14])=[C:6]([C:4]([OH:5])=[O:3])[CH:7]=[N:8]1)([CH3:19])[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 589728691-(2-hydroxy-1,1-dimethyl-ethyl)-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester

生成物 1

HCID 58972822HCID 58972822、化合物収率 95%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of 1-(2-hydroxy-1,1-dimethyl-ethyl)-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester (328 mg, 1.17 mmol) in methanol (5 mL) and water (5 mL) was added LiOH (34 mg, 1.4 mmol). The reaction mixture was stirred at reflux overnight, and then the solution was concentrated under reduced pressure to remove the methanol. The residue was diluted with water and the solution was acidified to pH=2 with concentrated HCl. The resulting mixture was then extracted with ethyl acetate three times. The combined organic extracts were concentrated in vacuo to give 1-(2-hydroxy-1,1-dimethyl-ethyl)-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid (280 mg, 95%), which was used without further purification.

後処理

  1. temperatureat reflux overnight
  2. concentrationthe solution was concentrated under reduced pressure
  3. customto remove the methanol
  4. additionThe residue was diluted with water
  5. extractionThe resulting mixture was then extracted with ethyl acetate three times
  6. concentrationThe combined organic extracts were concentrated in vacuo

出典と根拠

ORDレコード
ord-e223e57aa3bc46948cdcf3b0a4bc1443
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07728029B2

反応ノート

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