Formic Acid → 5-Methoxy-4-methylbenzimidazole

HRID 327450ノート

反応式

HRID 327450 の反応式
[CH3:1][O:2][C:3]1[C:4]([CH3:11])=[C:5]([NH2:10])[C:6]([NH2:9])=[CH:7][CH:8]=1.[CH:12](O)=O>>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]2[NH:9][CH:12]=[N:10][C:5]=2[C:4]=1[CH3:11]

参加物

3

反応物 2

HCID 284Formic AcidHCID 5924544-Methoxy-3-methylbenzene-1,2-diamine

生成物 1

HCID 199193885-Methoxy-4-methylbenzimidazole収率 84%

反応条件

温度
60 °C

実験手順

A mixture of 4-methoxy-3-methyl-1,2-benzenediamine (2.8 g, 18.4 mmol) and formic acid (30 mL) was heated at 60° C. for 30 minutes. The formic acid was removed under pressure and the product was partitioned between chloroform and water containing sufficient sodium hydroxide to basify the solution. After evaporation of the solvent the crude product was chromatographed (methanol:chloroform) to give 2.55 g (84%) of 5-methoxy-4-methyl-1H-benzimidazole.

後処理

  1. customThe formic acid was removed under pressure
  2. customthe product was partitioned between chloroform and water containing sufficient sodium hydroxide
  3. customAfter evaporation of the solvent the crude product
  4. customwas chromatographed (methanol:chloroform)

出典と根拠

ORDレコード
ord-fc36aca38dfe4222af2349fc7f21e98b
出典データセット
uspto-grants-1993_12
特許番号
US05273975

反応ノート

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