반응 #56318

ord-014ae2fa5ffd4701817a05d6204d0400

용매

반응 조건

온도
5°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타equipped with stirrer
  2. 2
    온도thermometer and cooling means
  3. 3
    workup.ADDITIONAfter the addition
  4. 4
    workup.STIRRINGstirring
  5. 5
    기타After this time the organic phase is separated from the aqueous phase
  6. 6
    여과is filtered
  7. 7
    세척The filtrate is then washed with aqueous sodium carbonate
  8. 8
    건조dried over anhydrous magnesium sulfate
  9. 9
    여과filtered

실험 절차

N-(4-Propyl-1,3-dioxolan-2-ylmethyl)-2-methoxyaniline (0.25 mole), diethyl ether (30 ml), sodium carbonate (35.5 grams) and water (50 ml) are charged into a glass reaction vessel equipped with stirrer, thermometer and cooling means. The mixture is cooled to about 5° C. and chloroacetyl chloride (0.28 mole) is added dropwise with stirring. After the addition is completed, stirring is continued for 1 hour. After this time the organic phase is separated from the aqueous phase and is filtered. The filtrate is then washed with aqueous sodium carbonate, dried over anhydrous magnesium sulfate and filtered. The filtrate is then stripped of solvent under reduced pressure to yield the desired product N-(4-propyl-1,3-dioxolan-2-ylmethyl)-2-methoxy-α-chloroacetanilide as the residue.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04225335uspto-grants-1980_09