HRID917396

反应详情

EQUATION

反应方程式

HRID 917396 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1.5 ml of butanol, 0.72 g (11 mmol) of 85.5% potassium hydroxide powder was suspended, followed by drop-wise adding, under ice-cooling, a 1.5 ml of butanol solution dissolving with 1.22 g (5.0 mmol) of ethyl 2-methansulfonyl-4-methylpyrimidine-5-carboxylate. After the end of the drop-wise addition, the solution was stirred at room temperature for 3 hours. To the reaction liquid, 50 ml of water was added, and the water layer was washed with diisopropyl ether, followed by adding 10% hydrochloric acid to make acidic, and extracting with ethyl acetate. The organic layer was washed with water and a saturated saline solution in this order, and dried over anhydrous magnesium sulfate. The solution was concentrated under reduced pressure to obtain 0.87 g (yield: 83%) of 2-butoxy-4-methylpyrimidine-5-carboxylic acid.

WORKUP

后处理

  1. additionadding, under ice-
  2. temperaturecooling
  3. additionAfter the end of the drop-wise addition
  4. additionwas added
  5. washthe water layer was washed with diisopropyl ether
  6. additionby adding 10% hydrochloric acid
  7. extractionextracting with ethyl acetate
  8. washThe organic layer was washed with water
  9. dry with materiala saturated saline solution in this order, and dried over anhydrous magnesium sulfate
  10. concentrationThe solution was concentrated under reduced pressure