반응 #982220

ord-13e1375b910e443da88378afdde20890

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux temperature
  2. 2
    기타The organic phase is separated
  3. 3
    세척washed neutral with water
  4. 4
    기타dried
  5. 5
    농축concentrated
  6. 6
    기타The solid residue is recrystallised from cyclohexane

실험 절차

81.5 g of 3,5-dichlorophenol and 2.5 g of diphenyl sulfide are dissolved in 1 liter of anhydrous ether. Then 2.5 g of anhydrous aluminium chloride are added and 80 g of bromine are added dropwise at room temperature in the course of 10 minutes. The reaction mixture is then stirred for 15 hours at reflux temperature and subsequently poured into water. The organic phase is separated, washed neutral with water, dried and concentrated. The solid residue is recrystallised from cyclohexane, affording 72.6 g of 3,5-dichloro-4-bromophenol in the form of colourless crystals with a melting point of 118°-120° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04285971uspto-grants-1981_08