m-Chloroperbenzoic acid → HCID 178493774、化合物

HRID 845514ノート

反応式

HRID 845514 の反応式
[CH3:1][O:2][C:3]1[C:8]([O:9][CH3:10])=[CH:7][N:6]=[C:5]([CH2:11][S:12][C:13]2[NH:17][C:16]3[CH:18]=[CH:19][C:20]([O:22][C:23]([F:28])([F:27])[CH:24]([F:26])[F:25])=[CH:21][C:15]=3[N:14]=2)[CH:4]=1.ClC1C=C(C=CC=1)C(OO)=[O:34]>C(Cl)Cl>[CH3:1][O:2][C:3]1[C:8]([O:9][CH3:10])=[CH:7][N:6]=[C:5]([CH2:11][S:12]([C:13]2[NH:17][C:16]3[CH:18]=[CH:19][C:20]([O:22][C:23]([F:27])([F:28])[CH:24]([F:25])[F:26])=[CH:21][C:15]=3[N:14]=2)=[O:34])[CH:4]=1

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 178493768HCID 178493768、化合物

生成物 1

HCID 178493774HCID 178493774、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of the product in methylene chloride is obtained by the procedure described in Example 2 by oxidation of 0.76 g of 2-[(4,5-dimethoxy-2-pyridyl)methylthio]-5-(1,1,2,2-tetrafluoroethoxy)-1H-benzimidazole with 19 ml of a 0.1M solution of m-chloroperoxybenzoic acid in 30 ml of methylene chloride at -40° C., after extraction. After drying the solution over magnesium sulfate, the drying agent is filtered off, the filtrate is concentrated and the residue is crystallized from methylene chloride/diisopropyl ether. 0.64 g (82% of theory) of the title compound is obtained in the form of colorless crystals of m.p. 160°-162° C. (decomp.).

後処理

  1. extractionafter extraction
  2. dry with materialAfter drying the solution over magnesium sulfate
  3. filtrationthe drying agent is filtered off
  4. concentrationthe filtrate is concentrated
  5. customthe residue is crystallized from methylene chloride/diisopropyl ether

出典と根拠

ORDレコード
ord-fb452fa10f6f47d1b71b3a9855095567
出典データセット
uspto-grants-1988_07
特許番号
US04758579

反応ノート

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