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Water → 5-Biphenyl-4-yl-6-fluoro-2-methanesulfonyl-1H-benzoimidazole

HRID 1960134
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HRID 1960134 반응식
[O-:1][Mn](=O)(=O)=O.[K+].[C:7]1([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH:12]=[CH:11][C:10]([C:13]2[C:23]([F:24])=[CH:22][C:16]3[NH:17][C:18]([S:20][CH3:21])=[N:19][C:15]=3[CH:14]=2)=[CH:9][CH:8]=1.[OH2:31]>C(O)(=O)C.CCOC(C)=O>[C:7]1([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH:12]=[CH:11][C:10]([C:13]2[C:23]([F:24])=[CH:22][C:16]3[NH:17][C:18]([S:20]([CH3:21])(=[O:1])=[O:31])=[N:19][C:15]=3[CH:14]=2)=[CH:9][CH:8]=1
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참가 물질

6

반응물 3

HCID 962WaterHCID 516875Potassium Permanganate2회HCID 673766005-Biphenyl-4-yl-6-fluoro-2-methylsulfanyl-1H-benzoimidazole

생성물 1

HCID 674455365-Biphenyl-4-yl-6-fluoro-2-methanesulfonyl-1H-benzoimidazole

시약·촉매·용매 2

HCID 176Acetic Acid용매2회
HCID 8857
Ethyl Acetate
용매

실험 절차

To 32 mL of acetic acid was added compound 13-5 (2.34, 6.4 mmol) resulting in a suspension. In a separate flask KMnO4 (2.48 g, 15.7 mmol) was dissolved in 40 mL of H2O. The KMnO4 solution was then added to the solution of compound 13-5 in acetic acid and allowed to stir for 2 h at ambient temperature. The dark reaction mixture was diluted with EtOAc (200 mL) and washed three times with 150 mL portions of brine. The combined organic layers were dried over MgSO4, then filtered and concentrated in vacuo to give title compound 13-6 as a pale yellow solid.

후처리

  1. customresulting in a suspension
  2. customThe dark reaction mixture
  3. washwashed three times with 150 mL portions of brine
  4. dry with materialThe combined organic layers were dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-179018b4bcba4b45b073333a238a45a2
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08410284B2

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