Benzene, 1-chloro-3-isocyanato- → Phenyl-(3-chlorophenylaminocarbonyloxy)-malonic acid diamide

HRID 255478

反応式

HRID 255478 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]=[C:9]=[O:10])[CH:5]=[CH:6][CH:7]=1.[C:11]1([C:17]([OH:24])([C:21]([NH2:23])=[O:22])[C:18]([NH2:20])=[O:19])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>C(OCC)(=O)C.CCCCCCCC([O-])=O.CCCCCCCC([O-])=O.[Zn+2]>[C:11]1([C:17]([O:24][C:9]([NH:8][C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[CH:3]=2)=[O:10])([C:21]([NH2:23])=[O:22])[C:18]([NH2:20])=[O:19])[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

参加物

5

反応物 2

HCID 17968Benzene, 1-chloro-3-isocyanato-HCID 131800612-Hydroxy-2-phenylmalonamide

生成物 1

HCID 13361940Phenyl-(3-chlorophenylaminocarbonyloxy)-malonic acid diamide収率 55.6%

試薬・触媒・溶媒 2

HCID 11180Zinc Caprylate触媒HCID 8857Ethyl Acetate溶媒

実験手順

0.5 g of zinc octoate and 4.45 g of 3-chlorophenyl isocyanate were added to 8.2 g of phenylhydroxymalonic acid diamide in 30 ml of ethyl acetate and the mixture was kept at 50° C. for 30 minutes. After cooling, the precipitate was filtered off with suction and recrystallised from acetone. 5.6 g of phenyl-(3-chlorophenylaminocarbonyloxy)-malonic acid diamide of melting point 196°-198° C. were obtained.

後処理

  1. temperatureAfter cooling
  2. filtrationthe precipitate was filtered off with suction
  3. customrecrystallised from acetone

出典と根拠

ORDレコード
ord-f4aee39cd75a4c03922b1961aa114d69
出典データセット
uspto-grants-1987_10
特許番号
US04698333

関連ノート

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