反応 #1955

ord-1ecb12c0a720485081b2a903dedaad68

反応方程式

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

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出the resultant aqueous mixture is extracted with methylene chloride
  2. 2
    乾燥The organic solution is dried over anhydrous magnesium sulfate
  3. 3
    ろ過filtered
  4. 4
    濃縮concentrated under reduced pressure
  5. 5
    workup.DISTILLATIONdistilled

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05726182uspto-grants-1998_03