Nitrone → 4-(2'-cyano-4'-bromo-6'-methylphenylazo)-N,N-diethylaniline

HRID 1701271

反応式

HRID 1701271 の反応式
Br[C:2]1[CH:7]=[C:6]([Br:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[N:10]=[N:11][C:12]1[CH:22]=[CH:21][C:15]([N:16]([CH2:19][CH3:20])[CH2:17][CH3:18])=[CH:14][CH:13]=1.[CH2:23]=[N:24]O.N1C(C)=CC=CC=1C.[N+](C1C=CC=CC=1)([O-])=O>[Cu]I>[C:23]([C:2]1[CH:7]=[C:6]([Br:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[N:10]=[N:11][C:12]1[CH:22]=[CH:21][C:15]([N:16]([CH2:19][CH3:20])[CH2:17][CH3:18])=[CH:14][CH:13]=1)#[N:24]

参加物

6

反応条件

温度
95 °C

実験手順

A stirred mixture of 4-(2',4'-dibromo-6'-methylphenylazo)-N,N-diethylaniline (4.25 parts), copper (I) iodide (2.0 parts), formaldoxime trimer (1.75 parts), 2,6-lutidine (2.15 parts), and nitrobenzene (150 parts) was heated to 95° C. for 6 hours when thin layer chromatography showed reaction to be complete. The mixture was cooled, filtered and the nitrobenzene was removed by steam distillation. Crystallisation of the solid product from ethanol gave 4-(2'-cyano-4'-bromo-6'-methylphenylazo)-N,N-diethylaniline (Found: C, 58.2; H, 5.4; Br, 21.7; N, 15.2. C18H19BrN4 requires C, 58.2; H, 5.15; Br, 21.55; N, 15.1%).

後処理

  1. customreaction
  2. temperatureThe mixture was cooled
  3. filtrationfiltered
  4. customthe nitrobenzene was removed by steam distillation
  5. customCrystallisation of the solid product from ethanol

出典と根拠

ORDレコード
ord-54d85bb108784b8bbeaa97feaa27ce35
出典データセット
uspto-grants-1980_03
特許番号
US04192800

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