HRID1869184

反应详情

EQUATION

反应方程式

HRID 1869184 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a RT suspension of N-methyl-3-phenyl-3-(1H-pyrrolo[2,3-b]pyridin-3-yl)-propionamide (54 mg, 0.19 mmol) in THF (5 ml) was added LiAlH4 (0.38 ml, 1M in THF) at room temperature. The resulting mixture was refluxed for 4 h, then the same amount of LiAlH4 was added. The resulting mixture was refluxed overnight, cooled to RT, quenched by addition of Na2SO4.10H2O. The mixture was stirred for 30 min and the solid was filtered off and washed with EtOAc. The filtrate was concentrated and purified via flash chromatography (DCM/MeOH/NH4OH) affording N-Methyl-[3-phenyl-3-(1H-pyrrolo[2,3-b]pyridin-3-yl)-propyl]amine as a white foam (28 mg, 56% yield); MS M+H=266.

WORKUP

后处理

  1. temperatureThe resulting mixture was refluxed for 4 h
  2. temperatureThe resulting mixture was refluxed overnight
  3. customquenched by addition of Na2SO4.10H2O
  4. filtrationthe solid was filtered off
  5. washwashed with EtOAc
  6. concentrationThe filtrate was concentrated
  7. custompurified via flash chromatography (DCM/MeOH/NH4OH)