HRID1916533

反应详情

EQUATION

反应方程式

HRID 1916533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

8.5 g (61.5 mmol) K2CO3 are added to a solution of 5.0 g (30.4 mmol) 3-(4-hydroxymethyl-phenyl)-propionaldehyde in 100 mL MeOH and then a solution of 7.0 g (36.4 mmol) dimethyl (1-diazo-2-oxo-propyl)-phosphonate in 50 mL MeOH is added dropwise and stirred for 3 h at RT. The reaction mixture is diluted with 200 mL EtOAc, washed with 80 mL saturated NaHCO3 solution, the aqueous phase extracted with 100 mL EtOAc and the combined organic phases are dried over Na2SO4. After the desiccant and solvent have been eliminated the residue is purified by chromatography on silica gel (cyc/EtOAc 3:1).

WORKUP

后处理

  1. washwashed with 80 mL saturated NaHCO3 solution
  2. extractionthe aqueous phase extracted with 100 mL EtOAc
  3. dry with materialthe combined organic phases are dried over Na2SO4
  4. customis purified by chromatography on silica gel (cyc/EtOAc 3:1)