HRID478203

反应详情

EQUATION

反应方程式

HRID 478203 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspended solution of 4-(3-indolyl)piperidine (48 mg, 0.24 mmol) and 1-(3-chloropropyl)-3-(4-methoxyphenyl)piperidine hydrochloride (61 mg, 0.2 mmol) in acetonitrile (13 mL) was added potassium carbonate (111 mg, 0.8 mmol), and the resulting mixture was refluxed for 12 hours. After the precipitated salt was filtered off, the filtrate was concentrated, and the resulting crude product was purified by column chromatography on a silica gel (eluent; chloroform:ammonia-saturated chloroform=10:1→3:1→1:2) to afford a free form (92 mg) of the title compound as a colorless viscous oil. After adding hydrochloric acid/methanol to a solution of the free form in methanol, the mixture was concentrated and was then freeze-dried to afford the title compound (81 mg, yield: 80%) as a white amorphous solid.

WORKUP

后处理

  1. temperaturethe resulting mixture was refluxed for 12 hours
  2. filtrationAfter the precipitated salt was filtered off
  3. concentrationthe filtrate was concentrated
  4. customthe resulting crude product was purified by column chromatography on a silica gel (eluent; chloroform:ammonia-saturated chloroform=10:1→3:1→1:2)