HRID1985220

反应详情

EQUATION

反应方程式

HRID 1985220 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-methyl-benzyl)-2-oxo-3-propyl-2,3-dihydro-1H-imidazol-4-yl]-ethyl ester (0.194 g, 1.51 mmol), 2-(4-hydroxy-phenoxy)-2-methyl-propionic acid ethyl ester (0.088 g, 0.392 mmol) and CS2CO3 (0.156 g, 0.478 mmol) in DMF (15 mL) was heated at 55° C. for under N2 for 16 h. The reaction mixture was cooled to room temperature, quenched with aqueous 1 N HCl (2 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 a gradient of 4:1 to 1:1 hexanes:acetone to afford 0.036 g (19%) 2-methyl-2-(4-{2-[1-(4-methyl-benzyl)-2-oxo-3-propyl-2,3-dihydro-1H-imidazol-4-yl]-ethoxy}-phenoxy)-propionic acid ethyl ester.

WORKUP

后处理

  1. customquenched with aqueous 1 N HCl (2 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