HRID26711

反应详情

EQUATION

反应方程式

HRID 26711 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. temperaturerefluxed for 1 hour
  2. customThe solvent was removed
  3. customby stripping under reduced pressure (15 mm.) at 50°
  4. customaffording the solid crude product
  5. customRecrystallization from a benzene-acetonitrile mixture