Water → 1,2-Diamino-4-(2,5-dimethoxyphenyl)-imidazole

HRID 357597ノート

反応式

HRID 357597 の反応式
[NH2:1][C:2]1[N:3]([N:17]=CC2C=CC=CC=2)[CH:4]=[C:5]([C:7]2[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[CH:9][C:8]=2[O:15][CH3:16])[N:6]=1.O.NN.O>C(O)COCCO>[NH2:17][N:3]1[CH:4]=[C:5]([C:7]2[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[CH:9][C:8]=2[O:15][CH3:16])[N:6]=[C:2]1[NH2:1]

参加物

5

反応物 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 539875062-Amino-1-benzylideneamino-4-(2,5-dimethoxyphenyl)-imidazole

生成物 1

HCID 189379581,2-Diamino-4-(2,5-dimethoxyphenyl)-imidazole

試薬・触媒・溶媒 1

HCID 8117Diethylene Glycol溶媒

実験手順

A solution of 26.1 g of 2-amino-1-benzylideneamino-4-(2,5-dimethoxyphenyl)-imidazole and 16.2 ml of hydrazine hydrate in 80 ml of diethylene glycol is stirred at 170° C. for 6 hours. After cooling, 400 ml of water are added to the reaction mixture. The product that has separated out is filtered off with suction, washed with water and recrystallized from 150 ml of ethanol. In that manner there is obtained the title compound, m.p. 159°-160° C., 1H-NMR (DMSO): δ=7.47 (d, 1H); 7.07 (s, 1H); 6.87 (d, 1H); 6.63 (q, 1H); 5.52 (s, 2H); 5.34 (s, 2H); 3.79 (s, 3H); 3.69 (s, 3H).

後処理

  1. temperatureAfter cooling
  2. customThe product that has separated out
  3. filtrationis filtered off with suction
  4. washwashed with water
  5. customrecrystallized from 150 ml of ethanol

出典と根拠

ORDレコード
ord-4bb20e6c8400459cb80b82418e6c800f
出典データセット
uspto-grants-1998_11
特許番号
US05840911

反応ノート

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