反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionadding, under ice-
- temperaturecooling
- additionAfter the end of the drop-wise addition
- additionwas added
- washthe water layer was washed with diisopropyl ether
- additionby adding 10% hydrochloric acid
- extractionextracting with ethyl acetate
- washThe organic layer was washed with water
- dry with materiala saturated saline solution in this order, and dried over anhydrous magnesium sulfate
- concentrationThe solution was concentrated under reduced pressure