HRID742482
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
- -78 °C
PROCEDURE
实验过程
To a solution of 1-triisoproylsilyl-pyrrole (13.2 g, 0.059 mol) in 250 mL of THF at -78° C. was added 10.45 g (0.0587 mol) of N-bromosuccinamide (NBS), and the mixture was stirred at -78° C. for 3 h. The reaction mixture was warmed to room temperature and concentrated in vacuo, and the resulting residue in hexane was stirred overnight. The hexane solution was filtered through alumina eluting with hexane, the eluate was concentrated in vacuo, and the residue was distilled (b.p. 107°-108° C./0.2 mm) to afford 10.4 g (58.4%) of 3-bromo-1-triisopropylsilyl-pyrrole.
WORKUP
后处理
- temperatureThe reaction mixture was warmed to room temperature
- concentrationconcentrated in vacuo
- stirringthe resulting residue in hexane was stirred overnight
- filtrationThe hexane solution was filtered through alumina eluting with hexane
- concentrationthe eluate was concentrated in vacuo
- distillationthe residue was distilled (b.p. 107°-108° C./0.2 mm)