HRID1775364
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
- 110 °C
PROCEDURE
实验过程
The residue of step A was dissolved in anhydrous THF (2 ml), Lawesson's reagent (40 mg, 0.2 mmol) was added and the mixture was stirred at 110° C. in closed vial under microwave heating. The mixture was concentrated under reduced pressure and the residue was purified by preparative HPLC (Waters X-Bridge, gradient of water containing 0.1% NH3 and acetonitrile) to yield 12 mg of a solid (0.039 mmol, yield 20% for two steps).
WORKUP
后处理
- temperatureheating
- concentrationThe mixture was concentrated under reduced pressure
- customthe residue was purified by preparative HPLC (Waters X-Bridge, gradient of water containing 0.1% NH3 and acetonitrile)