تفاعل #54989

ord-515cd4a944c94100a0ce420c1a056260

المذيبات

ظروف التفاعل

درجة الحرارة
25°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةrefluxed for 1 hour
  2. 2
    أخرىThe solvent was removed
  3. 3
    أخرىby stripping under reduced pressure (15 mm.) at 50°
  4. 4
    أخرىaffording the solid crude product
  5. 5
    أخرىRecrystallization from a benzene-acetonitrile mixture

الإجراء التجريبي

A mixture of 34 parts of N,N-dimethyl-2-hydroxyimino-3-methoxyiminobutyramide, 350 parts of methylene chloride, 13 parts of methyl isocyanate and one-tenth part triethylenediamine was stirred at 25° C. for 3 hours and then refluxed for 1 hour. The solvent was removed by stripping under reduced pressure (15 mm.) at 50° bath temperature, thereby affording the solid crude product. Recrystallization from a benzene-acetonitrile mixture gave 32 parts of N,N-dimethyl-3-methoxyimino-2-[(methylcarbamoyl)oximino]butyramide, m.p. 172°-173° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04151296uspto-grants-1979_04