HRID473059

反应详情

EQUATION

反应方程式

HRID 473059 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

To a suspension of LAH and THF was slowly charged (R)-(1-methylpyrrolidin-2-yl)(5-(2-(phenylsulfonyl)ethyl)-1H-indol-3-yl)methanone at 0° C. and then the reaction was slowly heated to reflux. Upon completion of the reaction in about 3-5 h, the reaction was cooled to 0-5° C. and 1N NaOH soln and H2O were sequentially charged. The solids were filtered and the precipitate washed with additional THF. The filtrate was distilled to dryness under reduced pressure. The residue was dissolved in water and the aqueous layer extracted with dichloromethane and dried over sodium sulfate and distilled to give the title compound in 75-80% yield.

WORKUP

后处理

  1. customat 0° C.
  2. temperaturethe reaction was slowly heated to reflux
  3. customUpon completion of the reaction in about 3-5 h
  4. filtrationThe solids were filtered
  5. washthe precipitate washed with additional THF
  6. distillationThe filtrate was distilled to dryness under reduced pressure
  7. dissolutionThe residue was dissolved in water
  8. extractionthe aqueous layer extracted with dichloromethane
  9. dry with materialdried over sodium sulfate
  10. distillationdistilled