HRID1617641

反应详情

EQUATION

反应方程式

HRID 1617641 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a suspension of 3-fluoro-4′-[3-(1-methyl-6-oxo-1,6-dihydro-pyridin-3-yl)-3-oxo-1-o-tolyl-propyl]-biphenyl-4-carboxylic acid methyl ester (35 mg) in THF (0.2 ml) and MeOH (0.2 ml) was added a 1M aqueous LiOH solution (0.145 ml) at 0° C. The mixture was stirred at 0° C. for 30 min and at room temperature for 1 h. Since the reaction was not finished, 1 M aqueous LiOH solution (0.435 ml) was added portionwise while stirring for another 24 h at room temperature. The reaction mixture was acidified using 1 M HCl. The organic solvents were removed under vacuum. The precipitated solid was collected by filtration, washed with water and dried to give the title compound (29 mg) as a colorless solid, MS (ESI−): m/z=468.2 [M−H]−.

WORKUP

后处理

  1. stirringwhile stirring for another 24 h at room temperature
  2. customThe organic solvents were removed under vacuum
  3. filtrationThe precipitated solid was collected by filtration
  4. washwashed with water
  5. customdried