HRID16401

反应详情

EQUATION

反应方程式

HRID 16401 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

539.7 g (2.35 mol) of 3-chloroperbenzoic acid are dissolved in 6.11 l of dichloromethane, and water that separates off is removed. The organic phase is dried over sodium sulfate and cooled to 0° C. A solution of 163 g (1.38 mol) of 1H-pyrrolo[2,3-b]pyridine in 1.00 l of dichloromethane is then added, and the temperature is allowed to increase to room temperature. After 2 hours, sufficient methanol to re-dissolve the precipitate formed is added. The mixture is filtered through silica gel (mobile phase: dichloromethane/methanol 95:5) and the product fractions are dried after concentration under high vacuum.

WORKUP

后处理

  1. customwater that separates off is removed
  2. dry with materialThe organic phase is dried over sodium sulfate
  3. temperatureto increase to room temperature
  4. customformed
  5. additionis added
  6. filtrationThe mixture is filtered through silica gel (mobile phase: dichloromethane/methanol 95:5)
  7. customthe product fractions are dried
  8. concentrationafter concentration under high vacuum