HRID1902254

反应详情

EQUATION

反应方程式

HRID 1902254 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 108.4 g (0.55 mol) of tryptaminehydrochloride in 1 liter of dry methanol and 93.2 g (0.68 mol) of methyl-3-chloropyruvate* was refluxed under N2 for 24 h. The cooled mixture was poured into brine, made basic with ammonium hydroxide and extracted with dichloromethane. Concentration and trituration with ethyl acetate gave 94.0 g (61.3%) of the chloromethyl tetrahydro-β-carboline, melting point ("mp") 123°-125° C. The product was recrystallized from dichloromethane/pentane.

WORKUP

后处理

  1. temperaturewas refluxed under N2 for 24 h
  2. extractionextracted with dichloromethane
  3. concentrationConcentration and trituration with ethyl acetate