HRID1628052
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
- 0 °C
PROCEDURE
实验过程
2-Bromo-6-(5-methoxy-1-methyl-1H-indol-3-yl)-5H-pyrrolo[2,3-b]pyrazine (0.500 g, 1.40 mmol; Preparation #B.1) in DMF (15 mL) was cooled to about 0° C. and then treated with 60 wt % NaH (0.112 g, 2.80 mmol). The mixture was stirred for about 15 min at about 0° C. followed by the addition of SEMCl (0.372 mL, 2.10 mmol). The mixture was warmed to rt for about 15 min then was concentrated under reduced pressure and purified on a 40 g silica gel column eluting with DCM to provide 2-bromo-6-(5-methoxy-1-methyl-1H-indol-3-yl)-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazine (0.61 g, 89%): LC/MS (Table 2, Method b) Rt=3.88 min; MS m/z 487 (M+H)+.
WORKUP
后处理
- temperatureThe mixture was warmed to rt for about 15 min
- concentrationthen was concentrated under reduced pressure
- custompurified on a 40 g silica gel column
- washeluting with DCM