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

HRID 27677

反応式

HRID 27677 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]I.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 88%

試薬・触媒・溶媒 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)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 (479 parts), copper (I) iodide (19 parts), anhydrous sodium acetate (246 parts), formamide (180 parts), acetic anhydride (408 parts) and n-butyl acetate (2190 parts) are mixed together and heated, with stirring, to 110° C. during 15 minutes. The temperature is maintained at 110° for 30 to 50 minutes, when a solid is suddenly precipitated from the reaction mixture, indicating completion of the reaction. The mixture is allowed to cool to room temperature and the product is collected, washed with ethanol to remove residual n-butyl acetate and dried. 2-Cyano-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino)azobenzene is obtained in 88% yield and requires no purification.

後処理

  1. temperatureheated
  2. temperatureThe temperature is maintained at 110° for 30 to 50 minutes
  3. customwhen a solid is suddenly precipitated from the reaction mixture
  4. customcompletion of the reaction
  5. temperatureto cool to room temperature
  6. customthe product is collected
  7. washwashed with ethanol
  8. customto remove residual n-butyl acetate
  9. customdried

出典と根拠

ORDレコード
ord-79b9351e6cbc4c129c78b56e06bd30c6
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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