1-Methyl-6-nitrobenzimidazole → 1-Methyl-1H-benzimidazol-6-amine

HRID 2375918노트

반응식

HRID 2375918 반응식
[CH3:1][N:2]1[C:6]2[CH:7]=[C:8]([N+:11]([O-])=O)[CH:9]=[CH:10][C:5]=2[N:4]=[CH:3]1>C(O)C.[Pd]>[CH3:1][N:2]1[C:6]2[CH:7]=[C:8]([NH2:11])[CH:9]=[CH:10][C:5]=2[N:4]=[CH:3]1

참가 물질

4

반응물 1

HCID 949781-Methyl-6-nitrobenzimidazole

생성물 1

HCID 136802831-Methyl-1H-benzimidazol-6-amine

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

Pd/C (17 mg, 10%, with 50% water) was added into the suspension of 1-methyl-6-nitro-1H-1,3-benzimidazole (85.0 mg, 0.480 mmol) in ethanol (3 mL). The mixture was degassed and filled with H2. The mixture was stirred at rt under balloon pressure for 16 h. After that time, the mixture was filtered and concentrated in vacuo to obtain the title compound as pink crystals. 1H NMR (CD3OD, 400 MHz): δ=3.67 (s, 3H), 6.69-6.73 (m, 2H), 7.33 (dd, 1H, J=0.4 & 8.8 Hz), 7.77 (s, 1H). MS (ES+): m/z 148.16 (100) [MH+]. HPLC: tR=0.43 min (ZQ2000, polar—5 min).

후처리

  1. customThe mixture was degassed
  2. additionfilled with H2
  3. filtrationAfter that time, the mixture was filtered
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-76e625f5be39408db0d54e25744bb982
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07465726B2

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