HRID2230314

反应详情

EQUATION

反应方程式

HRID 2230314 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the product from Example 24 (0.3 g, 0.63 mmol), 3-pyridylmethanol (0.061 mL, 0.63 mmol) and triphenylphosphine (0.165 g, 0.63 mmol) in 10 mL of tetrahydrofuran at 0° C. was treated with diethylazodicarboxylate (0.11 g, 0.63 mmol). The reaction mixture was warmed to room temperature and stirred for 4 hours. The reaction mixture was concentrated, and the residue was taken up in EtOAc and washed with sat. aqueous NaHCO3 and brine. The organic phase was dried with Na2SO4, filtered, and concentrated. The residue was purified by HPLC to give the title compound (0.047 g).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. washwashed with sat. aqueous NaHCO3 and brine
  3. dry with materialThe organic phase was dried with Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified by HPLC