تفاعل #3600

ord-0324d1ccc345444c9eb2d3d9fc2f1123

معادلة التفاعل

Nc1ccc(C(=O)N2Cc3ccc(Cl)n3Cc3ccccc32)cc1
3-chloro-10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine
CCN(CC)CC
triethylamine
Cc1ccccc1C(=O)Cl
2-methylbenzoylchloride
Cc1ccccc1C(=O)Nc1ccc(C(=O)N2Cc3ccc(Cl)n3Cc3ccccc32)cc1
N-[4-(3-Chloro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)ylcarbonyl)phenyl]-2-methylbenzamide

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلThe mixture is washed with water, and 1M NaHCO3 and dried(Na2 SO4)
  2. 2
    أخرىThe solvent is removed in vacuo
  3. 3
    أخرىto give a solid which
  4. 4
    أخرىis recrystallized from dichloromethane-hexane
  5. 5
    أخرىto give crystals, 185°-187° C.

الإجراء التجريبي

A mixture of 1 mmol of 3-chloro-10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 2 mmol of triethylamine, and 1.1 mmol of 2-methylbenzoylchloride in 8 ml of dichloromethane is stirred at room temperature overnight. The mixture is washed with water, and 1M NaHCO3 and dried(Na2 SO4). The solvent is removed in vacuo to give a solid which is recrystallized from dichloromethane-hexane to give crystals, 185°-187° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05733905uspto-grants-1998_03