HRID77510
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
A mixture of 60 mg (0.27 mmol) 3,5-diamino-6-chloro-N[(methylsulfanyl)methanimidoyl]-pyrazine-2-carboxamide (intermediate 3) and 60 mg (S)-3-amino-1-benzyl-piperidine in 2 ml THF is stirred at 70° C. overnight. Then the reaction mixture is concentrated under reduced pressure and the residue is purified by preparative reverse phase HPLC (gradient of acetonitrile and water+0.2% trifluoroacetic acid, 25° C.). Fractions containing the title compound were concentrated under reduced pressure treated with excess HCl in methanol and evaporated again.
WORKUP
后处理
- concentrationThen the reaction mixture is concentrated under reduced pressure
- customthe residue is purified by preparative reverse phase HPLC (gradient of acetonitrile and water+0.2% trifluoroacetic acid, 25° C.)
- additionFractions containing the title compound
- concentrationwere concentrated under reduced pressure
- additiontreated with excess HCl in methanol
- customevaporated again