HRID629870

反应详情

EQUATION

反应方程式

HRID 629870 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

1-(2,2-Dimethylpropyl)-5-[2-(4-methoxyphenyl)-6-methyl-2-azabicyclo-[2.2.2]oct-5-en-5-yl]-3-methyl-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (7-3, 40.3 mg, 0.09 mmol, 1.0 equiv) was added to CH3CN (820 μL) and water (820 μL). To this suspension was added aqueous H2SO4 (90 μL, 0.09 mmol, 1.0 equiv, 1.0 M) followed by periodic acid in one portion (21 mg, 0.09 mmol, 1.0 equiv). The reaction contents were heated to 50° C. for 18 h. Following this duration, LCMS showed consumption of starting material. The mixture was subsequently filtered through Celite, rinsed with CH3CN and purified by reverse-phase HPLC (15-90% CH3CN:0.1% TFA in H2O) to give 7-4 as a tan solid.

WORKUP

后处理

  1. customThe reaction contents
  2. customconsumption of starting material
  3. filtrationThe mixture was subsequently filtered through Celite
  4. washrinsed with CH3CN
  5. custompurified by reverse-phase HPLC (15-90% CH3CN:0.1% TFA in H2O)