Reacción #932311

ord-b3070be7085240f79907b62ae9cbb499

Condiciones de reacción

Temperatura
0°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.STIRRINGthe mixture is stirred for 30 minutes
  2. 2
    FiltraciónThe salt precipitate is collected by filtration
  3. 3
    Lavadothe filtrate is washed with two 200-ml portions of water
  4. 4
    Secadodried over anhydrous sodium sulfate
  5. 5
    workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
  6. 6
    workup.DISTILLATIONthe residue is further distilled under reduced pressure

Procedimiento

In 70 ml of dichloromethane are dissolved 13 ml of 2-methyl-1-butanol and 17 g of 1-chloroethyl chloroformate, and the solution is cooled to 0° C. With stirring, a solution of 9.6 ml of pyridine in 30 ml of dichloromethane is added dropwise, and the mixture is stirred for 30 minutes. The salt precipitate is collected by filtration and the filtrate is washed with two 200-ml portions of water and dried over anhydrous sodium sulfate. The solvent is then distilled off under reduced pressure and the residue is further distilled under reduced pressure to give 12.5 g of 1-chloroethyl 2-methylbutyl carbonate.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04755598uspto-grants-1988_07