Reacción #1801

ord-68830d19234b4026807695ab721a68e9

Ecuación de reacción

O=C=O
CO2
O=C(Cl)C(=O)Cl
oxalyl chloride
CN(C)C(=O)N(C)C
tetramethylurea
CN(C)C(Cl)=[N+](C)C.[Cl-]
Tetramethylchloroformamidinium chloride

Reactivos

Ninguno

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe reaction medium is maintained
  2. 2
    Otroformed by the reaction
  3. 3
    workup.DISTILLATIONThe CCl4 is then eliminated by distillation at atmospheric pressure

Procedimiento

A solution of 3.2 ml (0.037 mol) of oxalyl chloride in 30 ml of anhydrous carbon tetrachloride is added dropwise to a solution of 4.4 ml (0.037 mol) of tetramethylurea in 20 ml of anhydrous carbon tetrachloride with stirring. The reaction medium is maintained at reflux, with continued stirring, until the evolution of gases (CO and CO2) formed by the reaction has ceased. The CCl4 is then eliminated by distillation at atmospheric pressure. Tetramethylchloroformamidinium chloride is obtained in the form of a white solid (6.23 g). This solid is placed in solution at O° C. in 40 ml of anhydrous acetonitrile.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05726253uspto-grants-1998_03