반응 #61667

ord-eaa408e68e90459c97843c8f9c84f0bf

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도while cooling with ice
  2. 2
    workup.ADDITIONis poured onto ice
  3. 3
    추출extracted with dichloromethane
  4. 4
    세척The combined organic phases are washed with water
  5. 5
    기타dried
  6. 6
    workup.STIRRINGThe residue is stirred in diethyl ether

실험 절차

13.0 g (0.062 mol) ethyl (2-amino-6-methoxy-phenyl)-carbamate and 10.3 mL (0.074 mol) triethylamine in 100 mL dichloromethane are added to a solution of 8.20 mL (0.068 mol) trichloromethylchloroformate in 50 mL dichloromethane while cooling with ice. After 4 hours stirring at ambient temperature the reaction mixture is poured onto ice and extracted with dichloromethane. The combined organic phases are washed with water, dried and freed from the solvent. The residue is stirred in diethyl ether.

출처

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