HRID658060
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-cyano-2-(tetrahydro-pyran-4-yl)-vinyl]-phosphonic acid diethyl ester (7.45 g, 27.1 mmol) in methanol (200 mL) was added sodium borohydride (5 g, 135 mmol, 5 pellets), portion wise over 1.5 hours. The resulting mixture was stirred an additional 2 hours. The solvent was evaporated in vacuo to yield an oil, to which was added 0.1N NaOH and ethyl acetate. The layers were separated, and the organic layer was dried with MgSO4 and filtered. The solvent was removed to yield an oil which was purified via silica column chromatography (50% EtOAc/heptane) to yield an oil.
WORKUP
后处理
- customThe solvent was evaporated in vacuo
- customto yield an oil
- customThe layers were separated
- dry with materialthe organic layer was dried with MgSO4
- filtrationfiltered
- customThe solvent was removed
- customto yield an oil which
- customwas purified via silica column chromatography (50% EtOAc/heptane)
- customto yield an oil