HRID506851

反应详情

EQUATION

反应方程式

HRID 506851 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of [1-cyano-2-(tetrahydro-pyran-4-yl)-hex-5-enyl]-phosphonic acid diethyl ester (6.26 g, 19.0 mmol) in dichloromethane (211 mL), H2O (173 mL) and acetic acid (73 mL), was added tetrabutylammonium bromide (127 mg) followed by the portionwise addition of KMnO4. The resulting mixture was then stirred at room temperature overnight. The resulting viscous solution was cooled to 0° C., and NaHSO3 was added slowly until the mixture became clear. The layers were separated, and the organic layer was dried over magnesium sulfate, filtered, and concentrated to yield a residue. Heptanes was added, and the resulting mixture was concentrated to yield a residue.

WORKUP

后处理

  1. temperatureThe resulting viscous solution was cooled to 0° C.
  2. customThe layers were separated
  3. dry with materialthe organic layer was dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto yield a residue
  7. concentrationthe resulting mixture was concentrated
  8. customto yield a residue