Acetic Anhydride → 5-[(2-Methoxyphenyl)methylene]-2-thioxo-4-imidazolidinone

HRID 247873ノート

反応式

HRID 247873 の反応式
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH:5]=O.[NH:11]1[CH2:17][C:15](=[O:16])[NH:14][C:12]1=[S:13].C([O-])(=O)C.[Na+].C(OC(=O)C)(=O)C>O.C(O)(=O)C>[CH3:1][O:2][C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH:5]=[C:17]1[NH:11][C:12](=[S:13])[NH:14][C:15]1=[O:16]

参加物

7

反応物 4

HCID 7918Acetic AnhydrideHCID 86582-MethoxybenzaldehydeHCID 517045Sodium AcetateHCID 12740302-Thiohydantoin

生成物 1

HCID 30046725-[(2-Methoxyphenyl)methylene]-2-thioxo-4-imidazolidinone収率 85.4%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

A mixture of 2-methoxybenzaldehyde (2.5 g, 18 mmoles), 2-thiohydantoin (2.0 g, 17 mmoles), sodium acetate (4.0 g, 49 mmoles), acetic anhydride (1/2 ml), and acetic acid (15 ml) is stirred under an inert atmosphere and heated to reflux. After 1 hour the mixture is stirred into water (300 ml), and the precipitate is filtered off, rinsed with water three times and dried. The product is triturated in boiling methanol, filtered off, and dried to afford the pure product (3.4 g), mp 234°-235° C.

後処理

  1. temperatureheated to reflux
  2. filtrationthe precipitate is filtered off
  3. washrinsed with water three times
  4. customdried
  5. customThe product is triturated
  6. filtrationfiltered off
  7. customdried

出典と根拠

ORDレコード
ord-8b9237f1117c48a88cc8d77ebdb85c34
出典データセット
uspto-grants-1993_05
特許番号
US05208250

反応ノート

読み込み中…