반응 #61665

ord-5731544a9aa245a3966584cf36fb4237

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.DISTILLATIONThe solvent is distilled off
  2. 2
    workup.STIRRINGthe residue is stirred with isopropanol, during which time a yellow solid
  3. 3
    기타is precipitated

실험 절차

17.1 mL (0.141 mol) trichloromethylchloroformate are added dropwise at reflux temperature to a solution of 23.8 g (0.142 mol) 2-methoxy-6-nitro-phenylamine in 300 mL THF and then the mixture is stirred for 4 hours at this temperature. The solvent is distilled off and the residue is stirred with isopropanol, during which time a yellow solid is precipitated. Yield: 25.0 g (73%); mass spectroscopy: [M+H]+=241.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07429583B2uspto-grants-2008_09