HRID635225
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
A mixture of 3 g (11 mmoles) of the compound obtained in Example 5, 2.88 g (11 mmoles) of 6-fluoro-3-(4-piperidinyl)-benzo[d]isoxazole hydrochloride, 2.16 g (26 mmoles) of sodium bicarbonate and a catalytic amount of potassium iodide in 80 mL of acetonitrile was heated at reflux for 48 hours. The mixture was then allowed to cool, poured onto 100 mL of water and extracted with 100 mL of chloroform. The chloroform extract was washed with water, dried over sodium sulphate and evaporated. The residue obtained was suspended in ethyl ether, filtered and dried at vaccum to give 2 g of 7-[3-[4-(6-fluorobenzo[d]isoxazole-3-yl)piperidin-1-yl]propoxy]-2-(hydroxymethyl)-chromen-4-one in 40% yield.
WORKUP
后处理
- temperatureat reflux for 48 hours
- temperatureto cool
- extractionextracted with 100 mL of chloroform
- extractionThe chloroform extract
- washwas washed with water
- dry with materialdried over sodium sulphate
- customevaporated
- customThe residue obtained
- filtrationfiltered
- customdried at vaccum