m-Chloroperbenzoic acid → 4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyridine 1-oxide

HRID 45856

反応式

HRID 45856 の反応式
[CH3:1][O:2][C:3]1[CH:29]=[CH:28][C:6]([CH2:7][N:8]2[CH:12]=[C:11]([C:13]3[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=3)[C:10]([C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([N+:25]([O-:27])=[O:26])[CH:20]=3)=[N:9]2)=[CH:5][CH:4]=1.ClC1C=CC=C(C(OO)=[O:38])C=1>ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][N:8]2[CH:12]=[C:11]([C:13]3[CH:14]=[CH:15][N+:16]([O-:38])=[CH:17][CH:18]=3)[C:10]([C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([N+:25]([O-:27])=[O:26])[CH:20]=3)=[N:9]2)=[CH:28][CH:29]=1

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 671847354-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyridine

生成物 1

HCID 671844794-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyridine 1-oxide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

100 mg (0.26 mmol) of 4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]-pyridine were dissolved in 3 mL of dichloromethane and 80 mg (0.52 mmol) of m-chloroperbenzoic acid were added. The mixture was stirred at room temperature for 4 hours, diluted with the same solvent and washed with aqueous sodium hydrogenocarbonate. The organic layer was then dried over sodium sulphate and evaporated to afford, after crystallization from ethylacetate, 49 mg (47%) of the title compound.

後処理

  1. additiondiluted with the same solvent
  2. washwashed with aqueous sodium hydrogenocarbonate
  3. dry with materialThe organic layer was then dried over sodium sulphate
  4. customevaporated
  5. customto afford
  6. customafter crystallization from ethylacetate, 49 mg (47%) of the title compound

出典と根拠

ORDレコード
ord-ec5d241991e2448c85173f2a5e28df02
出典データセット
uspto-grants-2013_09
特許番号
US08541575B2

関連ノート

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