HRID626123

反应详情

EQUATION

反应方程式

HRID 626123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customquenched with water
  2. extractionextracted with EtOAc
  3. washThe extract was washed with water
  4. customdried
  5. concentrationconcentrated
  6. customto give a residue
  7. customthe white suspension thus formed
  8. customremoved
  9. filtrationfiltration
  10. concentrationThe filtrate was concentrated in vacuo
  11. customthe residue was purified by column chromatography (petroleum ether/CH2Cl2/acetone=4/2/1)