HRID2291564
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
1-Acetylpiperazine (6.23 g), 5-fluoro-2-nitrotoluene (7.51 g) and sodium carbonate (5.12 g) in dimethylformamide (40 ml) were stirred at 100° overnight, evaporated, and the residue partitioned between ethyl acetate and water. The organic layer was dried (sodium sulphate), evaporated, and the residue chromatographed over Merck (Trade Mark) t.l.c. grade silica, developing and eluting with 5% methanol in dichloromethane, yield 10.92 g of the title compound. A small portion was recrystallized from methanol/ethyl acetate, m.p. 133°-7°.
WORKUP
后处理
- customevaporated
- customthe residue partitioned between ethyl acetate and water
- dry with materialThe organic layer was dried (sodium sulphate)
- customevaporated
- customthe residue chromatographed over Merck (Trade Mark)
- washeluting with 5% methanol in dichloromethane, yield 10.92 g of the title compound
- customA small portion was recrystallized from methanol/ethyl acetate, m.p. 133°-7°