HRID2278663

反应详情

EQUATION

反应方程式

HRID 2278663 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
14 °C

PROCEDURE

实验过程

429 mg of sodium cyanoborohydride are added in portions to a solution of 490 mg of 4-(4-methylpiperazin-1-yl)-1H-indole, in 17 ml of acetic acid cooled to 14° C. The reaction medium is stirred for 2 hours at ambient temperature and then poured into a water/ice mixture and the pH is brought to neutrality with an aqueous ammonia solution. The mixture is then extracted with dichloromethane and the combined organic phases are dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The residue is purified by silica column chromatography, elution being carried out with a mixture of dichloromethane and methanol (95/05), so as to give 395 mg of 4-(4-methylpiperazin-1-yl)-2,3-dihydro-1H-indole in the form of a colorless viscous oil.

WORKUP

后处理

  1. extractionThe mixture is then extracted with dichloromethane
  2. dry with materialthe combined organic phases are dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe residue is purified by silica column chromatography, elution
  6. additionbeing carried out with a mixture of dichloromethane and methanol (95/05)