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

HRID 2375918ノート

反応式

HRID 2375918 の反応式
[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

参加物

4

反応物 1

HCID 949781-Methyl-6-nitrobenzimidazole

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-76e625f5be39408db0d54e25744bb982
出典データセット
uspto-grants-2008_12
特許番号
US07465726B2

反応ノート

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