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Trifluoroacetic acid → HCID 58046327、化合物

HRID 2359333
ノート
印刷プレビュー

反応式

HRID 2359333 の反応式
[Cl:1][C:2]1[C:3]([O:16][C:17]2[CH:22]=[CH:21][C:20]([O:23][C:24]([F:27])([F:26])[F:25])=[C:19]([Cl:28])[CH:18]=2)=[CH:4][C:5]([F:15])=[C:6]([CH:14]=1)[C:7]([O:9]C(C)(C)C)=[O:8].FC(F)(F)C(O)=O>ClCCl>[Cl:1][C:2]1[C:3]([O:16][C:17]2[CH:22]=[CH:21][C:20]([O:23][C:24]([F:25])([F:26])[F:27])=[C:19]([Cl:28])[CH:18]=2)=[CH:4][C:5]([F:15])=[C:6]([CH:14]=1)[C:7]([OH:9])=[O:8]
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 6422Trifluoroacetic acid2 回HCID 58046321HCID 58046321、化合物

生成物 1

HCID 58046327HCID 58046327、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Tert-butyl 5-chloro-4-[3-chloro-4-(trifluoromethoxy)phenoxy]-2-fluorobenzoate (Preparation 161, 41.88 g, 0.0868 mol) was dissolved in dichloromethane (75 mL), then trifluoroacetic acid (21.2 mL, 0.285 mol) was added and the mixture was stirred at room temperature for 50 hours. Trifluoroacetic acid was added again (1.2 mL, 0.017 mol) and the reaction left to stir for 4 hours. A solid was observed in the flask, so it was collected by filtration. The filtrate was concentrated in vacuo and dichloromethane (5 mL) was added to the crude, which was stirred for 5 minutes at room temperature. The resulting solid was collected by filtration and set aside. The crops were combined and title compound was isolated as a white solid (29.6 g, 81%).

後処理

  1. waitthe reaction left
  2. stirringto stir for 4 hours
  3. filtrationwas collected by filtration
  4. concentrationThe filtrate was concentrated in vacuo and dichloromethane (5 mL)
  5. additionwas added to the crude, which
  6. stirringwas stirred for 5 minutes at room temperature
  7. filtrationThe resulting solid was collected by filtration

出典と根拠

ORDレコード
ord-75df01c9b4f545fca2ba7299cb20a1c8
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08685977B2

反応ノート

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