HRID1946591
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 solution of (E)-2-chloro-11-(piperazin-1-yl)dibenzo[b,f][1,4]oxazepine (0.25 g, 0.8 mmol) and ethyl 2-(methylsulfonyl)pyrimidine-5-carboxylate (0.13 g, 0.57 mmol) in DME was stirred at room temperature for 1 h. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic extract was washed with saturated aqueous solution of bicarbonate, water, acetic acid and sodium acetate (pH=4), dried over sodium sulfate and solvent evaporated. The resulting crude residue was purified by flash chromatography (0% to 30% ethyl acetate in hexane) to afford title compound 116 (0.265 g, quant.).
WORKUP
后处理
- extractionextracted with ethyl acetate
- extractionThe organic extract
- washwas washed with saturated aqueous solution of bicarbonate, water, acetic acid and sodium acetate (pH=4)
- dry with materialdried over sodium sulfate and solvent
- customevaporated
- customThe resulting crude residue was purified by flash chromatography (0% to 30% ethyl acetate in hexane)