تفاعل #1801

ord-68830d19234b4026807695ab721a68e9

معادلة التفاعل

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

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction medium is maintained
  2. 2
    أخرىformed by the reaction
  3. 3
    workup.DISTILLATIONThe CCl4 is then eliminated by distillation at atmospheric pressure

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05726253uspto-grants-1998_03