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

HRID 53985

反応式

HRID 53985 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-3d0d18ea8fa64a2b90025bea52f01bed
出典データセット
uspto-grants-1997_04
特許番号
US05620991

関連ノート

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