HRID1985231

反应详情

EQUATION

反应方程式

HRID 1985231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-(4-{2-[1-(4-methoxy-benzyl)-3-methyl-2-oxo-imidazolidin-4-yl]-ethoxy}-phenoxy)-2-methyl-propionic acid ethyl ester (2.72 g, 5.78 mmol) and triethylsilane (1.34 g, 11.5 mmol) was treated with trifluoroacetic acid (70 mL) and stirred at room temperature under N2 for 5 h. The reaction mixture was diluted with water and then extracted with ethyl acetate. The organic layer was dried (MgSO4) and the solvent removed in vacuo to afford crude product that was purified by flash chromatography using 98:2 CH2Cl2:MeOH to afford 2.40 g (100%) 2-methyl-2-{4-[2-(3-methyl-2-oxo-imidazolidin-4-yl)-ethoxy]-phenoxy}-propionic acid ethyl ester. Rf=0.09 (1:1 hexanes:acetone); MS (ES+) Calc'd for C18H27N2O5 (M+1) 351. Found m/z 351 (100%). 1H NMR.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  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