반응 #3637

ord-635b45d2248548ecadd2ea29f0ad9ceb

반응 방정식

Cc1ccccc1C(=O)Cl
2-methylbenzoyl chloride
CCN(CC)CC
triethylamine
Nc1ccc(C(=O)N2Cc3ccnn3Cc3ccccc32)cc1
5,10-dihydro-5-(4-aminobenzoyl)-4H-pyrazolo-[5,1-c][1,4]benzodiazepine
Cc1ccccc1C(=O)Nc1ccc(C(=O)N2Cc3ccnn3Cc3ccccc32)cc1
desired product
Cc1ccccc1C(=O)Nc1ccc(C(=O)N2Cc3ccnn3Cc3ccccc32)cc1
N-[4-(4H-Pyrazolo[5,1-c][1,4]benzodiazepin-5(10H)-ylcarbonyl)phenyl]-2-methylbenzamide

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척is then washed with water, NaHCO3, and brine
  2. 2
    건조The organic layer is dried with Na2SO4
  3. 3
    여과filtered
  4. 4
    기타evaporated in vacuo
  5. 5
    기타to give a solid which
  6. 6
    기타is purified by flash chromatography on silica gel

실험 절차

To a stirred solution of 3 mmol of 2-methylbenzoyl chloride in 10 ml of methylene chloride is added 5 mmol of triethylamine and 3 mmol of 5,10-dihydro-5-(4-aminobenzoyl)-4H-pyrazolo-[5,1-c][1,4]benzodiazepine. The mixture is stirred at room temperature for 5 hours and is then washed with water, NaHCO3, and brine. The organic layer is dried with Na2SO4, filtered and evaporated in vacuo to give a solid which is purified by flash chromatography on silica gel to give the desired product as a solid, m.p. 142°-146° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05733905uspto-grants-1998_03