반응 #83443

ord-3b51b30d4d2046f4902a0548759eb3d1

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척The reaction mixture is washed with water
  2. 2
    건조the organic layer dried with Na2SO4
  3. 3
    workup.ADDITIONHexane is added at the boil

실험 절차

A solution of 0.83 g of 10,11-dihydro-10-(4-amino-3-methylbenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 0.5 g of N,N-diisopropylethylamine and 0.6 g of 2-methylbenzoyl chloride in 50 ml of methylene chloride is stirred at room temperature for 18 hours. The reaction mixture is washed with water, the organic layer dried with Na2SO4 and passed through a pad of hydrous magnesium silicate. Hexane is added at the boil to give 0.75 g of a solid which is crystallized from methylene chloride-hexane to give 0.61 g of the desired product, m.p. 125°-130° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05624923uspto-grants-1997_04