HRID1075566

反应详情

EQUATION

反应方程式

HRID 1075566 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

A mixture of 0.200 gm (0.74 mMol) 5-(N-[acetyl]amino)-3-(1-methylpiperidin-4-yl)pyrrolo[3,2-b]pyridine and 0.125 gm (3.31 mMol) lithium aluminum hydride in 40 mL tetrahydrofuran was heated at 75° C. for 18 hours. The reaction mixture was cooled to 0° C. and was then treated with sodium sulfate decahydrate. After vigorous stirring the reaction mixture was filtered through a pad of celite and the filtrate concentrated under reduced pressure. The residue was subjected to flash silica gel chromatography, eluting with dichloromethane containing from 0-20% methanol. Fractions containing product were combined and concentrated under reduced pressure to provide 0.10 gm (54%) of the title compound.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. filtrationwas filtered through a pad of celite
  3. concentrationthe filtrate concentrated under reduced pressure
  4. washeluting with dichloromethane containing from 0-20% methanol
  5. additionFractions containing product
  6. concentrationconcentrated under reduced pressure