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Trifluoroacetic acid → HCID 58046327, 화합물

HRID 2359333
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HRID 2359333 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acid2회HCID 58046321HCID 58046321, 화합물

생성물 1

HCID 58046327HCID 58046327, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-75df01c9b4f545fca2ba7299cb20a1c8
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08685977B2

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