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

HRID 1960134
ノート
印刷プレビュー

反応式

HRID 1960134 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 516875Potassium Permanganate2 回HCID 673766005-Biphenyl-4-yl-6-fluoro-2-methylsulfanyl-1H-benzoimidazole

生成物 1

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

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回
HCID 8857
Ethyl Acetate
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-179018b4bcba4b45b073333a238a45a2
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08410284B2

反応ノート

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