3,4-Diaminobenzonitrile → 2-(Chloromethyl)-1H-benzo[d]imidazole-6-carbonitrile

HRID 1901351ノート

反応式

HRID 1901351 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[NH2:10])[C:5]#[N:6].Cl.[Cl:12][CH2:13][C:14](=N)OCC>C(O)C>[Cl:12][CH2:13][C:14]1[NH:1][C:2]2[CH:3]=[C:4]([C:5]#[N:6])[CH:7]=[CH:8][C:9]=2[N:10]=1

参加物

4

反応物 2

HCID 7372853,4-DiaminobenzonitrileHCID 12470659Ethyl 2-chloroethanecarboximidate hydrochloride

生成物 1

HCID 218444532-(Chloromethyl)-1H-benzo[d]imidazole-6-carbonitrile収率 54.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

3.42 g of 3,4-diaminobenzonitrile and 4.06 g of ethyl chloroacetoimidate hydrochloride were dissolved in 100 ml of ethanol, and the solution was refluxed under heating for 3 hours. After cooling and distilling off the solvent, the resulting residue was dissolved in ethyl acetate, washed with water, and then dried. After distilling off the solvent, the crystals thus precipitated were collected by filtration to obtain 2.7 g of 2-chloromethyl-5-benzimidazolecarbonitrile.

後処理

  1. temperaturethe solution was refluxed
  2. temperatureunder heating for 3 hours
  3. temperatureAfter cooling
  4. distillationdistilling off the solvent
  5. dissolutionthe resulting residue was dissolved in ethyl acetate
  6. washwashed with water
  7. customdried
  8. distillationAfter distilling off the solvent
  9. customthe crystals thus precipitated
  10. filtrationwere collected by filtration

出典と根拠

ORDレコード
ord-9f0d54ad97a44a509a1348fd91dfa50f
出典データセット
uspto-grants-1996_11
特許番号
US05576343

反応ノート

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