HRID1944010

反应详情

EQUATION

反应方程式

HRID 1944010 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-5 °C

PROCEDURE

实验过程

To 0.47 mL (0.47 mmol) of a molar solution of LiAlH4 diluted in 1 mL of anhydrous THF, cooled to −5° C., is added dropwise by syringe a suspension of 190 mg (0.36 mmol) of N-[2-(ethyloxycarbonyl)imidazo[1,2-a]pyrid-7-yl]-5-trifluoromethyl-1-[(3-fluorophenyl)-methyl]-1H-indole-2-carboxamide, prepared according to the protocol described in step 17.3, in 4 mL of anhydrous THF. After stirring for 3 hours at room temperature, the reaction medium is poured slowly into a mixture (v/v) of water and concentrated sodium hydroxide, and is then extracted with 3×100 mL of dichloromethane. The combined organic phases are dried over magnesium sulfate and then concentrated under reduced pressure. The crude reaction product obtained is purified by chromatography on a column of silica, eluting with a mixture of dichloromethane and methanol. 30 mg of the expected product are thus obtained.

WORKUP

后处理

  1. additionis added dropwise by syringe
  2. customprepared
  3. extractionis then extracted with 3×100 mL of dichloromethane
  4. dry with materialThe combined organic phases are dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe crude reaction product
  7. customobtained
  8. customis purified by chromatography on a column of silica
  9. washeluting with a mixture of dichloromethane and methanol