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m-Chloroperbenzoic acid → 3-(1-(cyclohexyl(methyl)carbamoyl)-1H-imidazol-4-yl)pyridine 1-oxide

HRID 530301
ノート
印刷プレビュー

反応式

HRID 530301 の反応式
[CH:1]1([N:7]([CH3:21])[C:8]([N:10]2[CH:14]=[C:13]([C:15]3[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=3)[N:12]=[CH:11]2)=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.ClC1C=C(C=CC=1)C(OO)=[O:27]>C(Cl)(Cl)Cl>[CH:1]1([N:7]([CH3:21])[C:8]([N:10]2[CH:14]=[C:13]([C:15]3[CH:16]=[N+:17]([O-:27])[CH:18]=[CH:19][CH:20]=3)[N:12]=[CH:11]2)=[O:9])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]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 66554294N-cyclohexyl-N-methyl-4-(pyridin-3-yl)-1H-imidazole-1-carboxamide

生成物 1

HCID 468314763-(1-(cyclohexyl(methyl)carbamoyl)-1H-imidazol-4-yl)pyridine 1-oxide収率 48.3%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a stirred solution of N-cyclohexyl-N-methyl-4-(pyridin-3-yl)-1H-imidazole-1-carboxamide (90 mg, 0.317 mmol) in chloroform (5 mL) was added 3-chlorobenzoperoxoic acid (149 mg, 0.475 mmol) in one portion. The reaction was allowed to stir at room temperature for 20 h. TLC showed the reaction to be complete and the mixture was evaporated to dryness. The residue was triturated with ether and the resulting white crystals were filtered off and dried in air. Recrystallisation from hot isopropanol gave a white powder (46 mg, 46%).

後処理

  1. customthe reaction
  2. customthe mixture was evaporated to dryness
  3. customThe residue was triturated with ether
  4. filtrationthe resulting white crystals were filtered off
  5. customdried in air
  6. customRecrystallisation from hot isopropanol

出典と根拠

ORDレコード
ord-018791ce68784746babe848db5645b65
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09353082B2

反応ノート

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