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Methanol → 4-(Trifluoroacetylamino)benzoic acid

HRID 2380719
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HRID 2380719 반응식
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=1.CO.C(N(CC)CC)C.[F:20][C:21]([F:28])([F:27])[C:22](OCC)=[O:23]>CCOC(C)=O>[F:20][C:21]([F:28])([F:27])[C:22]([NH:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=1)=[O:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 9784-Aminobenzoic AcidHCID 8471TriethylamineHCID 9794Ethyl trifluoroacetate

생성물 1

HCID 2890744-(Trifluoroacetylamino)benzoic acid

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A solution of p-aminobenzoic acid in MeOH (500 mg, 3.65 mmol) was treated with 1.0 eq triethylamine (3.65 mmol, 509 μl) followed by 1.1 eq trifluoroacetic acid, ethyl ester (4.015 mmol, 478 μl). The solution was stirred overnight. The solution was diluted with EtOAc, washed with 5% KHSO4, followed by brine. The solution was dried over MgSO4 and solvent was removed by evaporation. The residue was purified by recrystallization in EtOAc/Hexane to afford eggshell-colored glossy plates (265 mg (31%), C9H6F3NO3).

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후처리

  1. washwashed with 5% KHSO4
  2. dry with materialThe solution was dried over MgSO4 and solvent
  3. customwas removed by evaporation
  4. customThe residue was purified by recrystallization in EtOAc/Hexane
  5. customto afford eggshell-colored glossy plates (265 mg (31%), C9H6F3NO3)

출처 및 근거

ORD 기록
ord-d57d20effe0840a0b5e26d243d4ec3a6
출처 데이터셋
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05369123

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