HRID658060

反应详情

EQUATION

反应方程式

HRID 658060 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvent was evaporated in vacuo
  2. customto yield an oil
  3. customThe layers were separated
  4. dry with materialthe organic layer was dried with MgSO4
  5. filtrationfiltered
  6. customThe solvent was removed
  7. customto yield an oil which
  8. customwas purified via silica column chromatography (50% EtOAc/heptane)
  9. customto yield an oil