Ethanol → 4,5-bis-(4-bromophenyl)-1H-imidazole-2-thione

HRID 1448983ノート

反応式

HRID 1448983 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([CH:10]([C:12]2[CH:17]=[CH:16][C:15]([Br:18])=[CH:14][CH:13]=2)O)=O)=[CH:4][CH:3]=1.[NH2:19][C:20]([NH2:22])=[S:21].O.C(O)C>C(O)CCCCC>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[NH:19][C:20](=[S:21])[NH:22][C:10]=2[C:12]2[CH:17]=[CH:16][C:15]([Br:18])=[CH:14][CH:13]=2)=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 702EthanolHCID 962WaterHCID 2723790ThioureaHCID 39382431,2-Bis(4-bromophenyl)-2-hydroxyethanone

生成物 1

HCID 35546154,5-bis-(4-bromophenyl)-1H-imidazole-2-thione

試薬・触媒・溶媒 1

HCID 81031-Hexanol溶媒

実験手順

A mixture of 4,4'-dibromobenzoin (25 g, 0.068 mol) and thiourea (10.3 g, 0.14 mol) in hexanol (200 ml) was refluxed with azeotropic distillation of water for three hours. The solution was then cooled and ethanol (300 ml) was added. The mixture was further cooled and the small needles which formed were collected and washed with cold ethanol then ether and dried. Recrystallization of the product from ethyl acetate gave 4,5-bis-(4-bromophenyl)-1H-imidazole-2-thione, m.p. 288°.

後処理

  1. temperatureThe solution was then cooled
  2. temperatureThe mixture was further cooled
  3. customthe small needles which formed
  4. customwere collected
  5. washwashed with cold ethanol
  6. dry with materialether and dried
  7. customRecrystallization of the product from ethyl acetate

出典と根拠

ORDレコード
ord-923517e0f45c4bbea8b8ddf7c9c5cb19
出典データセット
uspto-grants-1980_02
特許番号
US04188397

反応ノート

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