HRID376349

反应详情

EQUATION

反应方程式

HRID 376349 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2-hydroxy-2-methyl-1-(4-(methylsulfonyl)phenyl)propan-1-one (2.87 g, 11.8 mmol), ethyl hydrogen malonate (2.02 g, 15.3 mmol), CMC (6.51 g, 15.4 mmol) and DMAP (0.35 g, 2.8 mmol) was dissolved in 100 mL of CH2Cl2. The mixture was stirred for 14 h at room temperature, then DBU (4 mL, 27 mmol) was added, stirred 1 h, then partitioned between CH2Cl2 and 1M HCl. The organic layer was washed with brine, filtered through cotton and evaporated. Purification by flash chromatography (90% ether/Hex) provided 2.50 g of the title compound.

WORKUP

后处理

  1. stirringstirred 1 h
  2. custompartitioned between CH2Cl2 and 1M HCl
  3. washThe organic layer was washed with brine
  4. filtrationfiltered through cotton
  5. customevaporated
  6. customPurification by flash chromatography (90% ether/Hex)