HRID521228

反应详情

EQUATION

反应方程式

HRID 521228 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

To a reaction vial was added 4-{4-carbamoyl-3-[(2-fluoropyridin-4-yl)amino]-1H-pyrazol-1-yl}-4-(cyanomethyl)piperidinium trifluoroacetate (Intermediate #38-4) (0.020 g, 0.058 mmol), 1-ethyl-1H-imidazole-2-carbaldehyde (0.0072 g, 0.058 mmol), Na(OAc)3BH (0.062 g, 0.29 mmol), TFA (0.030 g, 0.26 mmol) suspended in DMF (0.97 mL). The reaction vessel was sealed and heated to 50° C. with stirring for 12 hours. The completed reaction was directly purified by reverse phase preparative HPLC (using a gradient elution of 0-95% ACN/water with 0.1% v/v NH4OH modifier) to afford the title compound, Example #22-1.

WORKUP

后处理

  1. customThe reaction vessel was sealed
  2. customThe completed reaction
  3. customwas directly purified by reverse phase preparative HPLC (
  4. washa gradient elution of 0-95% ACN/water with 0.1% v/v NH4OH modifier)