HRID369973

反应详情

EQUATION

反应方程式

HRID 369973 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension (+)-9-nitro-1,2,3,5,6,10b-hexahydropyrrolo[2,1-a]isoquinoline hydrochloride (1.83 g, 7.18 mmol) and 10% Pd-C (0.2 g) in ethanol (150 ml) was hydrogenated at 50 psi for 0.75 h. The solution was filtered and the filtrate was concentrated to a volume of 25 ml. It was then heated to reflux to dissolve all of the solid and upon cooling the product precipitated. The title compound was isolated as a white solid (1.37 g, 85%), m.p. 239-41.5° C.; [α]D +62.5° (c 1.13, MeOH). This salt was a single enantiomer by chiral CE.

WORKUP

后处理

  1. filtrationThe solution was filtered
  2. concentrationthe filtrate was concentrated to a volume of 25 ml
  3. temperatureIt was then heated
  4. temperatureto reflux
  5. dissolutionto dissolve all of the solid
  6. temperatureupon cooling the product
  7. customprecipitated