반응 #83501

ord-6fafba2a6afb4f6683c7f9417e124f59

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도is refluxed overnight
  2. 2
    세척The mixture is washed with saturated NaHCO3 solution
  3. 3
    건조dried (Na2SO4)
  4. 4
    세척the filter cake washed with dichloromethane
  5. 5
    농축The filtrate is concentrated
  6. 6
    workup.ADDITIONhexane added
  7. 7
    온도Chilling

실험 절차

A mixture of 8.26 g of ethyl 4-aminobenzoate, 8.26 g of N-chlorosuccinimide in 50 ml of dichloromethane is refluxed overnight. The mixture is washed with saturated NaHCO3 solution and dried (Na2SO4). The solution is passed through a thin pad of hydrous magnesium silicate and the filter cake washed with dichloromethane. The filtrate is concentrated and hexane added. Chilling gives 7.38 g of ethyl 3-chloro-4-aminobenzoate, m.p. 82°-83° C.

출처

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