반응 #2186178

ord-ad61beb158bb4b2e95dae3a756733df4

반응 방정식

CCOc1cccc(F)c1Cl
compound ( b43 )
CCOc1cccc(F)c1Cl
2-chloro-1-ethoxy-3-fluorobenzene
BrBr
bromine
CCOc1ccc(Br)c(F)c1Cl
1-bromo-3-chloro-4-ethoxy-2-fluorobenzene
수율 86.4%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added dropwise over 1 hour in a temperature range of 20 to 40° C.
  2. 2
    기타The resulting reaction mixture
  3. 3
    세척was washed with a saturated sodium thiosulfate aqueous solution
  4. 4
    기타The resulting reaction mixture
  5. 5
    세척having been washed
  6. 6
    workup.DISTILLATIONwas subjected to fractional distillation under reduced pressure

실험 절차

606 g of the compound (b43) was added to a reactor in a nitrogen atmosphere, to which 570 g of bromine was added dropwise over 1 hour in a temperature range of 20 to 40° C., followed by stirring for 30 minutes. The resulting reaction mixture was washed with a saturated sodium thiosulfate aqueous solution, a 10% sodium hydroxide aqueous solution, and water. The resulting reaction mixture having been washed was subjected to fractional distillation under reduced pressure to obtain 760 g of 1-bromo-3-chloro-4-ethoxy-2-fluorobenzene (C2). The resulting compound (C2) was white solid and had a melting point of 65.4 to 66.1° C. and a boiling point of 125 to 127° C./8 mmHg.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07569258B2uspto-grants-2009_08