HRID1985230

反应详情

EQUATION

反应方程式

HRID 1985230 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of toluene-4-sulfonic acid 2-[1-(4-methoxy-benzyl)-3-methyl-2-oxo-imidazolidin-4-yl]-ethyl ester (3.10 g, 7.41 mmol), 2-(4-hydroxy-phenoxy)-2-methyl-propionic acid ethyl ester (1.50 g, 6.69 mmol) and CS2CO3 (2.62 g, 8.04 mmol) in DMF (70 mL) was heated at 65° C. for under N2 for 16 h. The reaction mixture was cooled to room temperature, quenched with aqueous 1 N HCl (25 mL), and worked up extractively with EtOAc and water. The organic layer was dried (MgSO4) and the solvent removed in vacuo to afford crude product that was purified by flash chromatography using 5:1 hexanes:acetone to afford 2.92 g (93%) 2-(4-{2-[1-(4-methoxy-benzyl)-3-methyl-2-oxo-imidazolidin-4-yl]-ethoxy}-phenoxy)-2-methyl-propionic acid ethyl ester. MS (ES+) Calc'd for C36H47N2O6 (M+1) 603. Found m/z 603 (100%). 1H NMR.

WORKUP

后处理

  1. customquenched with aqueous 1 N HCl (25 mL)
  2. dry with materialThe organic layer was dried (MgSO4)
  3. customthe solvent removed in vacuo
  4. customto afford crude product that
  5. customwas purified by flash chromatography