HRID266421

反应详情

EQUATION

反应方程式

HRID 266421 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To E-2-hydroxyimino-N-methyl-2-(2-phenoxyphenyl)acetamide (10.00 g, 0.037 mole) were added acetone (200 ml), potassium carbonate (15.34 g, 0.111 moles) and dimethylsulfate (9.33 g, 0.074 moles) and the mixture was stirred at room temperature for 9 hours. After completion of the reaction, the reaction mixture was filtered, washed with acetone and concentrated under reduced pressure. The oil thus obtained was dissolved in toluene (50 ml) and to this was added an aqueous 1N sodium hydroxide solution (50 ml), followed by stirring at room temperature for 30 minutes. The mixture was extracted with toluene, washed with water and concentrated, and then the resulting residue was recrystallized (methanol/water) to obtain E-2-methoxyimino-N-methyl-2-(2-phenoxyphenyl)acetamide (9.93 g, yield: 94.4%) as colorless crystals (melting point: 81.5°-83° C.).

WORKUP

后处理

  1. customAfter completion of the reaction
  2. filtrationthe reaction mixture was filtered
  3. washwashed with acetone
  4. concentrationconcentrated under reduced pressure
  5. customThe oil thus obtained
  6. stirringby stirring at room temperature for 30 minutes
  7. extractionThe mixture was extracted with toluene
  8. washwashed with water
  9. concentrationconcentrated
  10. customthe resulting residue was recrystallized (methanol/water)