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Methanol → HCID 86692472、化合物

HRID 1748524
ノート
印刷プレビュー

反応式

HRID 1748524 の反応式
[OH-:1].[Na+].O.C([O:6][C:7]([C:9]1[CH:10]=[N:11][N:12]([C:15]2[C:20](F)=[CH:19][C:18]([C:22]([F:25])([F:24])[F:23])=[CH:17][N:16]=2)[C:13]=1[CH3:14])=[O:8])C.[CH3:26]O>O1CCCC1>[CH3:26][O:1][C:20]1[C:15]([N:12]2[C:13]([CH3:14])=[C:9]([C:7]([OH:6])=[O:8])[CH:10]=[N:11]2)=[N:16][CH:17]=[C:18]([C:22]([F:25])([F:24])[F:23])[CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 887MethanolHCID 962WaterHCID 14798Sodium HydroxideHCID 86692473HCID 86692473、化合物

生成物 1

HCID 86692472HCID 86692472、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4N Aqueous solution of sodium hydroxide (20 ml) and water (20 ml) were added to a solution of 1-[3-fluoro-5-(trifluromethyl)pyridin-2-yl]-5-methyl-1H-pyrazole-4-carboxylic acid ethyl ester (3 g) in methanol (20 ml) and tetrahydrofuran (20 ml), and stirred at room temperature for five hours. After completion of the reaction, the organic solvent was evaporated, diethylether and water was added to the residue. The aqueous layer was separated, pH was adjusted to 5 by the addition of concentrated hydrochloric acid under ice cooling, and the precipitated solid was collected by filtration dried at 60° C. under air blow to give the titled compound (1.17 g) as a white solid.

後処理

  1. customAfter completion of the reaction
  2. customthe organic solvent was evaporated
  3. additiondiethylether and water was added to the residue
  4. customThe aqueous layer was separated
  5. additionpH was adjusted to 5 by the addition of concentrated hydrochloric acid under ice cooling
  6. filtrationthe precipitated solid was collected by filtration
  7. customdried at 60° C. under air blow

出典と根拠

ORDレコード
ord-1a7dfa76143b42e49c9e21b3c8f67bd6
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09150555B2

反応ノート

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