Reacción #1060239

ord-90f57a94ef5d49eda773f547c70aa463

Disolventes

Condiciones de reacción

Temperatura
60°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroInto a 100 ml four-necked flask there were placed
  2. 2
    Otroat room temperature
  3. 3
    TemperaturaAfter cooling
  4. 4
    Lavadothe reaction solution was washed with water
  5. 5
    Secadothe benzene layer was dried over anhydrous sodium sulfate
  6. 6
    Otrothe benzene was removed under reduced pressure
  7. 7
    OtroThe residue obtained
  8. 8
    workup.DISTILLATIONwas distilled under reduced pressure

Procedimiento

Into a 100 ml four-necked flask there were placed 17.8 g of N-(3-chloroallyl)glycine ethyl ester, 15.2 g of triethylamine and 50 ml of benzene, and then 16.9 g of γ-chlorobutyryl chloride was gradually dropwise added thereto at room temperature with thorough stirring. Thereafter, the mixture was stirred for 1 hour at 60° C. After cooling, the reaction solution was washed with water, the benzene layer was dried over anhydrous sodium sulfate and the benzene was removed under reduced pressure. The residue obtained was distilled under reduced pressure to obtain 23.7 g of the objective N-(3-chloroallyl)-N-γ-chlorobutyryl glycine ethyl ester (b.p.2 167 - 170° C, nD23.0 1.4884).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04054668uspto-grants-1977_10