반응 #70272

ord-a4e2c39a7efe46fa98d2f35b3345c17e

반응 방정식

O=[N+]([O-])c1cnc(O)c(Br)c1
3-bromo-5-nitropyridin-2-ol
O=P(Br)(Br)Br
POBr3
BrP(Br)Br
PBr3
O=[N+]([O-])c1cnc(Br)c(Br)c1
expected product
수율 73.0%
O=[N+]([O-])c1cnc(Br)c(Br)c1
2,3-dibromo-5-nitropyridine
수율 73.0%

용매

반응 조건

온도
120°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with DCM
  2. 2
    기타The crude mixture was purified by flash chromatography over SiO2 eluting with hexane/ethyl acetate

실험 절차

A mixture of 3-bromo-5-nitropyridin-2-ol, POBr3 and PBr3 was heated at 120° C. for 3.5 h. The crude mixture was poured into a mixture of ice and water and extracted with DCM. The crude mixture was purified by flash chromatography over SiO2 eluting with hexane/ethyl acetate mixtures affording 2.63 g (yield 73%) of the expected product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08536165B2uspto-grants-2013_09