HRID1292988
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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A mixture of 4-chloro-2-fluoro-nitrobenzene (28.5 mmol), 1-methylpiperazine (28.5 mmol) and K2CO3 (37.0 mmol) in DMF is stirred at 100° C. for 16 h and diluted with water and EtOAc. The phases are separated and the aqueous phase is extracted with EtOAc. The organic phase and the extracts are combined, washed sequentially with water and brine, dried over Na2SO4 and dried in vacuo. The resultant residue is chromatographed (silica gel, 10% methanol in EtOAc as eluent) to afford the title product.
WORKUP
后处理
- customThe phases are separated
- extractionthe aqueous phase is extracted with EtOAc
- washwashed sequentially with water and brine
- dry with materialdried over Na2SO4
- customdried in vacuo
- customThe resultant residue is chromatographed (silica gel, 10% methanol in EtOAc as eluent)