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m-Chloroperbenzoic acid → HCID 54274875、化合物

HRID 1900184
ノート
印刷プレビュー

反応式

HRID 1900184 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[F:12][C:13]1[CH:18]=[CH:17][C:16]([S:19][CH2:20][CH:21]([NH:23][C:24](=[O:36])[C@H:25]([CH:33]([CH3:35])[CH3:34])[NH:26][C:27]([O:29][CH:30]([CH3:32])[CH3:31])=[O:28])[CH3:22])=[CH:15][CH:14]=1>C(Cl)Cl>[F:12][C:13]1[CH:18]=[CH:17][C:16]([S:19]([CH2:20][CH:21]([NH:23][C:24](=[O:36])[C@H:25]([CH:33]([CH3:35])[CH3:34])[NH:26][C:27]([O:29][CH:30]([CH3:31])[CH3:32])=[O:28])[CH3:22])=[O:9])=[CH:15][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 53780799HCID 53780799、化合物

生成物 1

HCID 54274875HCID 54274875、化合物収率 69%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1.3 g of m-chloroperbenzoic acid was added to a solution containing 2.5 g of N1 -[2-(4-fluorophenylthio)-1-methylethyl]-N2 -isopropoxycarbonyl-L-valinamide dissolved in 50 ml of methylene chloride, at 0° C. After the mixture was stirred for 5 hours at room temperature, the reaction mixture was filtered. The filtrate was washed successively with a saturated aqueous solution of potassium carbonate and water, the organic layer was dried over anhydrous sodium sulfate and the methylene chloride was removed under reduced pressure. The obtained residue was purified by column chromatography on silica gel, thus obtaining 1.8 g of the desired product in the form of a colorless prism-shaped crystal (yield: 69%).

後処理

  1. filtrationthe reaction mixture was filtered
  2. washThe filtrate was washed successively with a saturated aqueous solution of potassium carbonate and water
  3. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  4. customthe methylene chloride was removed under reduced pressure
  5. customThe obtained residue was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-94f328faf1bb4cb2a47113c58509d247
出典データセット
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05574064

反応ノート

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