HRID1058090

反应详情

EQUATION

反应方程式

HRID 1058090 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 2l three necked, round bottom flask, 500 ml dimethylformamide is added, followed by addition of 100 g of 2-(N-methyl-N-(2-pyridyl)amino)ethanol (II) and 100 g of 4-fluorobenzaldehyde (III) was added to the reaction mixture and it was stirred for 10 minutes at room temperature and 80 g of potassium tertiary butoxide was added to the reaction mixture. The reaction was monitored by TLC. After completion of the reaction, the reaction mixture was cooled to 5-10° C. and under the cold conditions, 1.5 l of water was added and stirred for 15 min. The mixture was extracted with 4×500 ml of ethyl acetate. The combined organic layer was washed with 3×1 l water. The organic layer was dried over anhydrous sodium sulphate and concentrated under reduced pressure to give 148 g (88%) of 4-[2-(N-methyl-N-(2-pyridyl)amino)ethoxy)benzaldehyde (IV).

WORKUP

后处理

  1. additionwas added to the reaction mixture and it
  2. customAfter completion of the reaction
  3. additionwas added
  4. stirringstirred for 15 min
  5. extractionThe mixture was extracted with 4×500 ml of ethyl acetate
  6. washThe combined organic layer was washed with 3×1 l water
  7. dry with materialThe organic layer was dried over anhydrous sodium sulphate
  8. concentrationconcentrated under reduced pressure