HRID1070460

反应详情

EQUATION

反应方程式

HRID 1070460 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a suspension of N-(4-hydroxy-2-methyl-6-quinolyl)acetamide (100 g, 0.46 mol) obtained in Preparation Example 1-1, Step 2 in toluene (490 ml) was added dimethyl sulfate (75 ml, 0.79 mol) and the mixture was refluxed under heating for 8 hr. The resulting precipitate was collected by filtration, dissolved in water (1350 ml) and heated to 70° C. The solution was filtered and 35% aqueous sodium hydroxide solution (100 ml) was added to the filtrate. The resulting precipitate was collected by filtration to give N-(4-methoxy-2-methyl-6-quinolyl)acetamide (55.3 g, 52%, pale-brown crystals).

WORKUP

后处理

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 8 hr
  3. filtrationThe resulting precipitate was collected by filtration
  4. dissolutiondissolved in water (1350 ml)
  5. filtrationThe solution was filtered
  6. addition35% aqueous sodium hydroxide solution (100 ml) was added to the filtrate
  7. filtrationThe resulting precipitate was collected by filtration