HRID1591659

反应详情

EQUATION

反应方程式

HRID 1591659 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

36.1 g (133 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboxamide from example 2C) are dissolved in 330 ml of THF, and 27 g (341 mmol) of pyridine are added. Then, over the course of 10 min, 47.76 ml (71.66 g, 341 mmol) of trifluoroacetic anhydride are added, during which the temperature rises to 40° C. The mixture is stirred at room temperature overnight. It is then added to 11 of water and extracted three times with 0.51 of ethyl acetate each time. The organic phase is washed with saturated sodium bicarbonate solution and with 1 N HCl, dried with MgSO4 and concentrated in a rotary evaporator.

WORKUP

后处理

  1. customrises to 40° C
  2. extractionextracted three times with 0.51 of ethyl acetate each time
  3. washThe organic phase is washed with saturated sodium bicarbonate solution and with 1 N HCl
  4. dry with materialdried with MgSO4
  5. concentrationconcentrated in a rotary evaporator