HRID642744

反应详情

EQUATION

反应方程式

HRID 642744 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred solution of compound 1F in dioxane (50 mL) and 2M KH2PO4 (50 mL) was added NaBH4 (1.0 g, 26.4 mmol) over a 10 min-period, and the stirring was continued at RT for 1 hr. The reaction mixture was diluted with 2M HCl to adjust pH to 1, and stirred at RT for another 1 hr. The reaction was concentrated, dissolved in EtOAc, washed with water, dried over Na2SO4, and concentrated. Purification by silica gel chromatography (50% EtOAc in hexanes) provided the title compound (1.9 g) as a pale yellow oil.

WORKUP

后处理

  1. concentrationThe reaction was concentrated
  2. dissolutiondissolved in EtOAc
  3. washwashed with water
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. customPurification by silica gel chromatography (50% EtOAc in hexanes)