HRID655264

反应详情

EQUATION

反应方程式

HRID 655264 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

In a N2 charged round bottom flask, Sodium Hydride, 60%, (41 mg, 1.01 mmol) was suspended in dimethylformamide (2.5 mL). The solution was maintained under N2 and cooled to 0° C. for 10 minutes. Next, 6-(1-Methyl-1H-pyrazol-4-yl)-1H-pyrrolo[3,2-b]pyridine (200 mg, 1.01 mmol) was dissolved in dimethylformamide (2.5 mL) and added to the cooled solution dropwise. The solution was allowed to stir at 0° C. for an additional 10 minutes. Finally, Bromo-acetic acid ethyl ester (123 uL, 1.11 mmol) was slowly added to the reaction vessel. The reaction was allowed to equilibrate back to room temperature, while stirring for 2 hours. Finally, the solution was transferred to a separatory funnel with dichloromethane (75 mL) and washed with water (2×75 mL). The organic layer was dried over Na2SO4, concentrated down and purified by flash chromatography (0-10% Methanol/dichloromethane step gradient) to afford the title compound (122 mg, 43% yield). MS m/z=285 [M+H+]+

WORKUP

后处理

  1. temperatureThe solution was maintained under N2
  2. additionadded to the cooled solution dropwise
  3. customto equilibrate back to room temperature
  4. stirringwhile stirring for 2 hours
  5. washwashed with water (2×75 mL)
  6. dry with materialThe organic layer was dried over Na2SO4
  7. concentrationconcentrated down
  8. custompurified by flash chromatography (0-10% Methanol/dichloromethane step gradient)