HRID553507

反应详情

EQUATION

反应方程式

HRID 553507 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve {2-[3′-(4-fluoro-phenyl)-2,3,5,6-tetrahydro-[1,2′]bipyrazinyl-4-yl]-ethyl}-methyl-amine (0.032 g, 0.101 mmol) in dichloromethane (5 mL). Add triethylamine (16 μL, 0.209 mmol) followed by 1-methyl-1H-imidazole-4-sulfonyl chloride (0.020 g, 0.112 mmol) and stir at ambient temperature for 72 hr. Concentrate under reduced pressure and purify (silica gel chromatography, eluting with 20:80 to 0:100 hexanes:ethyl acetate, then 10:90 methanol:ethyl acetate, then 20:80 methanol:ethyl acetate) to give the free base of the title compound (23 mg, 50%).

WORKUP

后处理

  1. concentrationConcentrate under reduced pressure
  2. custompurify (silica gel chromatography
  3. washeluting with 20:80 to 0:100 hexanes