m-Chloroperbenzoic acid → 2-(Benzenesulfinyl)-4,5-bis(4-methoxyphenyl)-1H-imidazole

HRID 370776ノート

反応式

HRID 370776 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH3:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[N:21]=[C:22]([S:33][C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)[NH:23][C:24]=2[C:25]2[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=2)=[CH:16][CH:15]=1>ClCCl>[CH3:12][O:13][C:14]1[CH:15]=[CH:16][C:17]([C:20]2[N:21]=[C:22]([S:33]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)=[O:9])[NH:23][C:24]=2[C:25]2[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=2)=[CH:18][CH:19]=1

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 12832306HCID 12832306、化合物

生成物 1

HCID 128323292-(Benzenesulfinyl)-4,5-bis(4-methoxyphenyl)-1H-imidazole収率 83%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 2.164 g of 3-chloroperbenzoic acid (80%) in 150 ml of dichloromethane is added dropwise to a solution of 3.89 g of 4,5-bis(4-methoxyphenyl)-2-phenylthioimidazole in 100 ml of dichloromethane. The mixture is stirred for 3 hours at room temperature, the solution is washed with sodium bicarbonate solution, dried over sodium sulfate, and concentrated to dryness under vacuum. The residue is crystallized from ether/hexane. Recrystallization from ether/hexane yields 3.36 g of 4,5-bis(4-methoxyphenyl)-2-phenylsulfinylimidazole, mp 188°-190°.

後処理

  1. washthe solution is washed with sodium bicarbonate solution
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated to dryness under vacuum
  4. customThe residue is crystallized from ether/hexane
  5. customRecrystallization from ether/hexane

出典と根拠

ORDレコード
ord-ff1ee996fe974b288e053f2eaccd5d97
出典データセット
uspto-grants-1985_07
特許番号
US04528298

反応ノート

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