반응 #524792

ord-054609431cda4882a1a5d0fc4bcd9d80

반응 방정식

C/C=C/C(=O)Cl
Crotonyl chloride
O=[N+]([O-])c1cc(Cl)cc(Cl)c1O
2,4-dichloro-6-nitrophenol
C/C=C/C(=O)Oc1c(Cl)cc(Cl)cc1[N+](=O)[O-]
2,4-dichloro-6-nitrophenyl crotonate

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture was heated
  2. 2
    온도under reflux for 12 hours
  3. 3
    추출extracted several times with a 10% sodium hydroxide solution
  4. 4
    세척The organic layer was washed with water
  5. 5
    건조dried (Na2SO4)
  6. 6
    기타the solvent removed under reduced pressure
  7. 7
    기타to give a pale brown oil which
  8. 8
    기타crystallised

실험 절차

Crotonyl chloride (7 ml) was added to a solution of 2,4-dichloro-6-nitrophenol (10.3 g) in methylene chloride (20 ml) and the mixture was heated under reflux for 12 hours. The solution was diluted with further methylene chloride (200 ml) and extracted several times with a 10% sodium hydroxide solution. The organic layer was washed with water dried (Na2SO4) and the solvent removed under reduced pressure to give a pale brown oil which crystallised on standing for 24 hours 2,4-dichloro-6-nitrophenyl crotonate melted at <60°.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04031249uspto-grants-1977_06