HRID857112

反应详情

EQUATION

反应方程式

HRID 857112 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 3-(3-{4-[(6-{benzyl[(2R)-2-(2,2-dimethyl-4H-1,3-benzodioxin-6yl)-2-hydroxyethyl]amino}hexyl)oxy]but-1-ynyl}phenyl)imidazolidine-2,4-dione (9.05 g) in a mixture of isopropanol-EtOAc (9:1, 200 ml) was hydrogenated over Pearlman's catalyst (1.8 g). After 2 days aqueous 2M HCl (10 ml) was added and the mixture was hydrogenated for a further 2 h. The catalyst was removed by filtration and the filtrate was concentrated under reduced pressure. The residue was purified by chromatography on Biotage eluting with dichloromethane-isopropanol-880 ammonia (34:7:1) to give the title compound (2.8 g) LCMS RT=2.34 min ES+ve 514 (MH)+.

WORKUP

后处理

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue was purified by chromatography on Biotage
  4. washeluting with dichloromethane-isopropanol-880 ammonia (34:7:1)