HRID1396861

反应详情

EQUATION

反应方程式

HRID 1396861 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 (2R)-2-(hydroxymethyl)-N-[(phenylmethyl)oxy]hexanamide (6) (52 g, 0.21 mol) and Ph3P (60 g, 0.23 mol) in THF (1500 mL) at 0° C. was added DIAD (41.8 g, 0.21 mol). The mixture was warmed up to rt and stirred overnight. TLC indicated completion of the reaction. THF was removed under vacuum. The residue was titurated with ethyl acetate/petroleum ether (1:10) and filtered. The filtrate was concentrated and the residue was purified by flash column chromatography to provide the title compound (52.8 g, 110%). LCMS: (M+H)+: 234.2.

WORKUP

后处理

  1. customcompletion of the reaction
  2. customTHF was removed under vacuum
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated
  5. customthe residue was purified by flash column chromatography