Formamide → Acetamide, N-(2-(2-(2-cyano-4,6-dinitrophenyl)diazenyl)-5-(diethylamino)phenyl)-

HRID 27681

反応式

HRID 27681 の反応式
Br[C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[C:3]=1[N:14]=[N:15][C:16]1[CH:21]=[CH:20][C:19]([N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])=[CH:18][C:17]=1[NH:27][C:28](=[O:30])[CH3:29].C([O-])(=O)C.[Na+].[CH:36]([NH2:38])=O.C(OC(=O)C)(=O)C>[Cu](Cl)Cl.C(OCCCC)(=O)C>[C:36]([C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[C:3]=1[N:14]=[N:15][C:16]1[CH:21]=[CH:20][C:19]([N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])=[CH:18][C:17]=1[NH:27][C:28](=[O:30])[CH3:29])#[N:38]

参加物

7

反応物 4

HCID 713FormamideHCID 7918Acetic AnhydrideHCID 104287Acetamide, N-[2-[2-(2-bromo-4,6-dinitrophenyl)diazenyl]-5-(diethylamino)phenyl]-HCID 517045Sodium Acetate

生成物 1

HCID 90383Acetamide, N-(2-(2-(2-cyano-4,6-dinitrophenyl)diazenyl)-5-(diethylamino)phenyl)-収率 96%

試薬・触媒・溶媒 2

HCID 24014Cupric Chloride触媒HCID 31272Butyl Acetate溶媒

反応条件

温度
110 °C

実験手順

2-Bromo-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino)azobenzene (2.4 parts), copper (II) chloride (0.67 parts), anhydrous sodium acetate (1.2 parts), formamide (1.8 parts), acetic anhydride (2.0 parts) and n-butyl acetate (44 parts) are mixed together and heated, with stirring, to 110° C. during 15 minutes. The temperature is maintained for 5 hours after which time the reaction is complete. The mixture is cooled to room temperature and poured into petroleum-ether (boiling range 60-80°) (400 parts). The precipitate is collected, washed with petroleum-ether (100 parts) and dried. 2-Cyano-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino)azobenzene is obtained in 96% yield.

後処理

  1. temperatureheated
  2. temperatureThe temperature is maintained for 5 hours after which time the reaction
  3. temperatureThe mixture is cooled to room temperature
  4. customThe precipitate is collected
  5. washwashed with petroleum-ether (100 parts)
  6. customdried

出典と根拠

ORDレコード
ord-a9221bcf0bbb4c9692966241d39232ec
出典データセット
uspto-grants-1980_09
特許番号
US04222935

関連ノート

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