반응 #1955

ord-1ecb12c0a720485081b2a903dedaad68

반응 방정식

O
water
Cc1cc(Cl)c(F)cn1
4-chloro-5-fluoro-2-picoline
Cc1cc(Cl)c(F)cn1
product
Cc1cc(Cl)c(F)cn1
4-Chloro-5-fluoro-2-picoline
CC(C)(C)OCl
t-butylhypochlorite
Cc1ncc(F)c(Cl)c1Cl
title compound
Cc1ncc(F)c(Cl)c1Cl
3,4-Dichloro-5-fluoro-2-picoline

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출the resultant aqueous mixture is extracted with methylene chloride
  2. 2
    건조The organic solution is dried over anhydrous magnesium sulfate
  3. 3
    여과filtered
  4. 4
    농축concentrated under reduced pressure
  5. 5
    workup.DISTILLATIONdistilled

실험 절차

To 0.87 g (6 mmol) of 4-chloro-5-fluoro-2-picoline, the product of Example 66, in 20 mL of chloroform cooled to -45° C., is added 0.75 mL of t-butylhypochlorite. The reaction mixture is stirred at -45° C. for 2 hours and at 0° C. for 2 hours. The reaction mixture is then poured into water and the resultant aqueous mixture is extracted with methylene chloride. The organic solution is dried over anhydrous magnesium sulfate, filtered, concentrated under reduced pressure and distilled to afford the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05726182uspto-grants-1998_03