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1,1'-Carbonyldiimidazole → 5-(4-Fluorophenyl)-4-[4-(methylsulfonyl)phenyl]thiophene-2-acetamide

HRID 1899079
ノート
印刷プレビュー

反応式

HRID 1899079 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:12][C:11]([CH2:13][C:14](O)=[O:15])=[CH:10][C:9]=2[C:17]2[CH:22]=[CH:21][C:20]([S:23]([CH3:26])(=[O:25])=[O:24])=[CH:19][CH:18]=2)=[CH:4][CH:3]=1.C(N1C=CN=C1)([N:29]1C=CN=C1)=O.O.N>O1CCCC1.O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:12][C:11]([CH2:13][C:14]([NH2:29])=[O:15])=[CH:10][C:9]=2[C:17]2[CH:22]=[CH:21][C:20]([S:23]([CH3:26])(=[O:25])=[O:24])=[CH:19][CH:18]=2)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 682631,1'-CarbonyldiimidazoleHCID 117947425-(4-Fluorophenyl)-4-[4-(methylsulfonyl)phenyl]thiophene-2-acetic acidHCID 12896473Azane;hydrate

生成物 1

HCID 233727565-(4-Fluorophenyl)-4-[4-(methylsulfonyl)phenyl]thiophene-2-acetamide収率 78.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

A mixture of 5-(4-fluorophenyl)-4-[4-(methylsulfonyl)phenyl]thiophene-2-acetic acid (4.1 g) and 1,1'-carbonyldiimidazole (1.8 g) in tetrahydrofuran (50 ml) was stirred and refluxed for 1 hour. The mixture was added dropwise to an ice-cooled mixture of ammonia water (28%; 5 ml) and tetrahydrofuran (10 ml). The resulting mixture was stirred overnight, diluted with water, and extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium bicarbonate, water, and dilute hydrochloric acid, successively. The organic layer was dried and concentrated, and the residue was recrystallized from a mixture of chloroform, ethyl acetate and ethanol to give crystals of 5-(4-fluorophenyl)-4-[4-(methylsulfonyl)phenyl]thiophene-2-acetamide (3.2 g).

後処理

  1. temperaturerefluxed for 1 hour
  2. temperaturecooled
  3. stirringThe resulting mixture was stirred overnight
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with an aqueous solution of sodium bicarbonate, water, and dilute hydrochloric acid
  6. customThe organic layer was dried
  7. concentrationconcentrated
  8. customthe residue was recrystallized from a mixture of chloroform, ethyl acetate and ethanol

出典と根拠

ORDレコード
ord-1a409b6469864cf28d5d9634197eee70
出典データセット
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05571810

反応ノート

読み込み中…

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