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m-Chloroperbenzoic acid → HCID 9822781、化合物

HRID 1736408
ノート
印刷プレビュー

反応式

HRID 1736408 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH:12]=[CH:11][N:10]=[C:9]1[S:13][CH2:14][CH2:15][CH2:16][O:17][C:18]1[CH:19]=[C:20]2[C:25](=[CH:26][CH:27]=1)[NH:24][C:23](=[O:28])[CH2:22][CH2:21]2.ClC1C=CC=C(C(OO)=[O:37])C=1>ClCCl>[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH:12]=[CH:11][N:10]=[C:9]1[S:13]([CH2:14][CH2:15][CH2:16][O:17][C:18]1[CH:19]=[C:20]2[C:25](=[CH:26][CH:27]=1)[NH:24][C:23](=[O:28])[CH2:22][CH2:21]2)=[O:37]
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 10668289HCID 10668289、化合物

生成物 1

HCID 9822781HCID 9822781、化合物収率 56.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In 1 liter of dichloromethane was dissolved 67 g of 6-{3-[1-(2-methylphenyl)-2-imidazolylthio]propoxy}-3,4-dihydrocarbostyril. Thereto was added 32.6 g of m-chloroperbenzoic acid with ice-cooling. The mixture was stirred overnight. After the completion of the reaction, the reaction mixture was washed five times with an aqueous solution saturated with sodium hydrogencarbonate, dried with magnesium sulfate, and subjected to distillation to remove the solvent. The residue was purified by a silica gel column chromatography (eluant: dichloromethane/ethyl acetate/methanol=30/10/1). The crude crystals were recrystallized from ethanol-n-hexane to obtain 39.5 g of 6-{3-[1-(2-methylphenyl)-2-imidazolylsulfinyl]propoxy}-3,4-dihydrocarbostyril.

後処理

  1. temperaturecooling
  2. customAfter the completion of the reaction
  3. washthe reaction mixture was washed five times with an aqueous solution saturated with sodium hydrogencarbonate
  4. dry with materialdried with magnesium sulfate
  5. distillationsubjected to distillation
  6. customto remove the solvent
  7. customThe residue was purified by a silica gel column chromatography (eluant: dichloromethane/ethyl acetate/methanol=30/10/1)
  8. customThe crude crystals were recrystallized from ethanol-n-hexane

出典と根拠

ORDレコード
ord-a6a14bfac77f4b859839f5e9037b2ac6
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05541198

反応ノート

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