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Potassium Hydroxide → 5-(3-(Aminomethyl)-2,6-dimethylphenyl)-2-(4-(trifluoromethyl)phenyl)-2H-1,2,4-triazol-3(4H)-one

HRID 59356
ノート
印刷プレビュー

反応式

HRID 59356 の反応式
[F:1][C:2]([F:32])([F:31])[C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:13](=[O:14])[NH:12][C:11]([C:15]3[C:16]([CH3:30])=[C:17]([CH:26]=[CH:27][C:28]=3[CH3:29])[CH2:18][NH:19]C(=O)C(F)(F)F)=[N:10]2)=[CH:5][CH:4]=1.[OH-].[K+]>C1COCC1>[NH2:19][CH2:18][C:17]1[C:16]([CH3:30])=[C:15]([C:11]2[NH:12][C:13](=[O:14])[N:9]([C:6]3[CH:7]=[CH:8][C:3]([C:2]([F:31])([F:32])[F:1])=[CH:4][CH:5]=3)[N:10]=2)[C:28]([CH3:29])=[CH:27][CH:26]=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 14797Potassium HydroxideHCID 136246060N-(3-(1-(4-(trifluoromethyl)phenyl)-4,5-dihydro-5-oxo-1H-1,2,4-triazol-3-yl)-2,4-dimethylbenzyl)-2,2,2-trifluoro acetamide

生成物 1

HCID 1364924295-(3-(Aminomethyl)-2,6-dimethylphenyl)-2-(4-(trifluoromethyl)phenyl)-2H-1,2,4-triazol-3(4H)-one収率 31.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of N-(3-(1-(4-(trifluoromethyl)phenyl)-4,5-dihydro-5-oxo-1H-1,2,4-triazol-3-yl)-2,4-dimethylbenzyl)-2,2,2-trifluoro acetamide (Example-106, 0.800 g, 1.74 mmol) in THF (10 mL), aqueous solution of KOH was added and the reaction mass was stirred at RT for 3-4 h. After completion of the reaction, the reaction mass was quenched with water and extracted with ethyl acetate. The organic layer was separated, dried over anhydrous sodium sulphate and concentrated to afford 0.200 g of the desired product. MS (m/z): 362.86 (M+H)+.

後処理

  1. customAfter completion of the reaction
  2. customthe reaction mass was quenched with water
  3. extractionextracted with ethyl acetate
  4. customThe organic layer was separated
  5. dry with materialdried over anhydrous sodium sulphate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-e922a3dc1d29414c949fc8e3ddd84471
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09439890B2

反応ノート

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