HRID2067163

反应详情

EQUATION

反应方程式

HRID 2067163 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of methyl 4-[({[2-chloro-5-({[3-(methyloxy)phenyl]methyl}oxy)phenyl]carbonyl}amino)methyl]benzoate (106 mg, 0.24 mmol) and lithium hydroxide (2 eq, 20 mg, 0.48 mmol) in dioxane (3 ml) and H2O (1.5 ml) was heated at 65° C. for 3 hours. On cooling solvent was evaporated in vacuo, residue acidified with 2M HCl and filtered to give the title compound as a white solid. MS (ES+) m/z 426 [M+H]+ (C23H2035ClNO5). 1H-NMR (400 MHz, d6-DMSO) δ 3.76 (3H, s), 4.50 (2H, d, J 6), 5.12 (2H, s), 6.91 1H, dd, J 1.6, J 7.6), 7.02 (1H, s), 7.09 (2H, m), 7.30 (1H, t, J 4), 7.40-7.47 (2H, m), 7.92 (2H, d, J 8), 9.04 (1H, t, J 6)

WORKUP

后处理

  1. temperatureOn cooling solvent
  2. customwas evaporated in vacuo, residue
  3. filtrationfiltered