HRID1382853
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 23 g (0.0163 mol) o-fluorobenzonitrile, 70 g (0.4889 mol) of 1,4-dioxa-8-azaspiro[4.5]decane, 34 g (0.246 mol) of K2CO3, and 150 ml of acetonitrile is stirred at reflux for three days. The reaction mixture is allowed to cool to ambient temperature, diluted with water and extracted with methylene chloride. The combined extracts are washed with brine, dried over Na2SO4, and concentrated in vacuo to give an oil. Trituration with ether furnishes 15.6 g (39%) of title compound: IR (KBr) 2200, 1590 and 1485 cm-1 ; NMR (CDCl3) δ7.65-6.9 (m, 4H), 4.02 (s, 4H), 3.33 (m, 4H), and 1.94 (m, 4H).
WORKUP
后处理
- temperatureat reflux for three days
- extractionextracted with methylene chloride
- washThe combined extracts are washed with brine
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo
- customto give an oil