HRID847161

反应详情

EQUATION

反应方程式

HRID 847161 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

10 g (74 mmol) of 1-methoxy-cyclopropane-carbonyl chloride are added at 20° C. with stirring to a mixture of 8 g (82 mmol) of N,O-dimethyl-hydroxylamine hydrochloride and 100 ml of absolute dichloromethane. 13 g (164 mmol) of absolute pyridine are then added dropwise at 0° C. The mixture is initially subsequently stirred at 20° C. for one hour and then at 40° C. for one hour, the precipitate is then filtered off and 100 ml of dichloromethane are added. The reaction mixture is washed with water, dried over sodium sulphate and concentrated by stripping off the solvent under reduced pressure. The remaining residue is subjected to a vacuum distillation. 10 g (85% of theory) of N-methoxy-N-methyl-1-methoxy-cyclopropanecarboxamide are obtained in this manner in the form of an oil having a boiling point of b.p.=125° C. at 20 mbar. ##STR35##

WORKUP

后处理

  1. waitat 40° C. for one hour
  2. filtrationthe precipitate is then filtered off
  3. addition100 ml of dichloromethane are added
  4. washThe reaction mixture is washed with water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated
  7. distillationThe remaining residue is subjected to a vacuum distillation