HRID270643
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
13.0 g of the compound obtained in Example 1 was dissolved in 260 mL of methanol, and a solution obtained by dissolving 4.84 g of sodium hydroxide in 26 mL of water was added thereto. The resulting solution was refluxed for 4 hours, cooled to room temperature, concentrated under reduced pressure to remove methanol. The resulting aqueous solution was washed with 10 ml of diethyl ether and acidified to pH 2 to 3 using concentrated HCl. The solids thus solidified were filtered, washed with a small amount of cold water and dried at 40° C. to obtain 9.60 g (yield of 85%) of the title compound as a brown solid.
WORKUP
后处理
- customa solution obtained
- additionwas added
- temperatureThe resulting solution was refluxed for 4 hours
- concentrationconcentrated under reduced pressure
- customto remove methanol
- washThe resulting aqueous solution was washed with 10 ml of diethyl ether
- filtrationThe solids thus solidified were filtered
- washwashed with a small amount of cold water
- customdried at 40° C.