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

HRID 357597노트

반응식

HRID 357597 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8117Diethylene Glycol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-4bb20e6c8400459cb80b82418e6c800f
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840911

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