HRID626123
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 tert-butyl 3-(methylsulfonyloxy)pyrrolidine-1-carboxylate (0.6 g, 2.26 mmol), bis(4-hydroxyphenyl)methanone (2.15 g, 10.0 mmol) and K2CO3 (313 mg, 2.26 mmol) in 12 mL DMF was heated at 100° C. for 3.5 h, then quenched with water, and extracted with EtOAc. The extract was washed with water, dried, and concentrated to give a residue, to which was added CH2Cl2 and the white suspension thus formed removed and filtration. The filtrate was concentrated in vacuo and the residue was purified by column chromatography (petroleum ether/CH2Cl2/acetone=4/2/1) to give the desired product (400 mg, 46% yield).
WORKUP
后处理
- customquenched with water
- extractionextracted with EtOAc
- washThe extract was washed with water
- customdried
- concentrationconcentrated
- customto give a residue
- customthe white suspension thus formed
- customremoved
- filtrationfiltration
- concentrationThe filtrate was concentrated in vacuo
- customthe residue was purified by column chromatography (petroleum ether/CH2Cl2/acetone=4/2/1)