반응 #62785

ord-8acb45df98e14c3a9a8f3a881c597456

반응 방정식

O=C(Cl)C(Cl)(Cl)Cl
Trichloroacetyl chloride
COCCNCC=CCl
N-(3-chloro)allyl-N-methoxyethylamine
CCN(CC)CC
triethylamine
COCCN(CC=CCl)C(=O)C(Cl)(Cl)Cl
above-named product
수율 92.7%
COCCN(CC=CCl)C(=O)C(Cl)(Cl)Cl
N-(3-chloro)allyl-N-methoxyethyl trichloroacetamide
수율 92.7%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction was kept at approximately 5° C. with an ice-water bath
  2. 2
    workup.ADDITIONUpon completion of the addition
  3. 3
    세척The reaction mixture was then washed twice with saturated brine
  4. 4
    건조dried with sodium sulfate
  5. 5
    기타Rotary evaporation

실험 절차

N-(3-chloro)allyl-N-methoxyethylamine (2.25 g, 0.015 mol) and 1.52 g (0.015 mol) triethylamine were stirred in 70 ml dichloromethane. The reaction was kept at approximately 5° C. with an ice-water bath. Trichloroacetyl chloride (2.73 g, 0.015 mol) in 10 ml dichloromethane was added dropwise to the cooled solution. Upon completion of the addition, the mixture was stirred at room temperature for 6 hours. The reaction mixture was then washed twice with saturated brine and dried with sodium sulfate. Rotary evaporation yielded 4.1 g of the above-named product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04762548uspto-grants-1988_08