HRID1456310
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
PROCEDURE
实验过程
To a solution of 1-(3-[1,3]dioxolan-2-yl-4-methoxy-phenyl)-1H-tetrazole (9.09 g) in dry tetrahydrofuran (200 ml) at -78° under nitrogen, n-butyl lithium solution in hexane (30 ml of 1.6 mol dm-3) was added. Nitrogen gas was evolved. After stirring under nitrogen for 5 min the mixture was allowed to warm to 0° over 10 min and 8% aqueous sodium bicarbonate (200 ml) was then added. After stirring for 10min ethyl acetate (150 ml) was added and the layers separated. The aqueous layer was then extracted with dichloromethane (2×200 ml) and the organic layers combined, dried (Na2SO4) and evaporated in vacuo to yield the title compound as an oil (8.0 g).
WORKUP
后处理
- temperatureto warm to 0° over 10 min
- additionwas added
- customthe layers separated
- extractionThe aqueous layer was then extracted with dichloromethane (2×200 ml)
- dry with materialdried (Na2SO4)
- customevaporated in vacuo