反応 #62785

ord-8acb45df98e14c3a9a8f3a881c597456

反応方程式

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
収率 92.7%
COCCN(CC=CCl)C(=O)C(Cl)(Cl)Cl
N-(3-chloro)allyl-N-methoxyethyl trichloroacetamide
収率 92.7%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The reaction was kept at approximately 5° C. with an ice-water bath
  2. 2
    workup.ADDITIONUpon completion of the addition
  3. 3
    洗浄The reaction mixture was then washed twice with saturated brine
  4. 4
    乾燥dried with sodium sulfate
  5. 5
    その他Rotary evaporation

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04762548uspto-grants-1988_08