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

HRID 361919

반응식

HRID 361919 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-be5bbb8febf3467ba171a1886efac5d3
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05866577

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