HRID1985153

反应详情

EQUATION

反应方程式

HRID 1985153 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-{4-[2-(1-Benzyl-3-methyl-2-oxo-imidazolidin-4-yl)-ethoxy]-phenyl}-2-butoxy-2-methyl-propionic acid ethyl ester and 5N NaOH (0.3 mL) in ethanol (3 mL) is refluxed under nitrogen for 1 h, cooled to ambient temperature, and concentrated. The residue is diluted with 1N HCl, extracted with CH2Cl2, dried, concentrated, and purified by LCMS to provide the title compound. 1H NMR (400 MHz, CDCl3): δ 7.33-7.22 (m, 5H), 7.07 (d, 2H, J=8.6 Hz), 6.71 (d, 2H, J=8.6 Hz), 4.39, 4.35 (ABq, 2H, J=15.3 Hz), 3.94 (t, 2H, J=5.7 Hz), 3.69-3.62 (m, 1H), 3.58-3.52 (m, 1H), 3.50-3.44 (m, 1H), 3.40 (t, 1H, J=9.1 Hz), 3.04-3.01 (m, 1H), 3.02, 2.94 (ABq, 2H, J=13.9 Hz), 2.85 (s, 3H), 2.25-2.18 (m, 1H), 1.92-1.85 (m, 1H), 1.62-1.54 (m, 1H), 1.46 (s, 3H), 1.42-1.32 (m, 2H), 0.92 (t, 3H, J=7.2 Hz). MS [EI+] 469 (M+H)+, [EI−] 467 (M−H)+.

WORKUP

后处理

  1. concentrationconcentrated
  2. additionThe residue is diluted with 1N HCl
  3. extractionextracted with CH2Cl2
  4. customdried
  5. concentrationconcentrated
  6. custompurified by LCMS