HRID660633

反应详情

EQUATION

反应方程式

HRID 660633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of PPh3-resin (5 g, 6.5 mmol) in methylene chloride (50 mL) at 0° C. is added iodine (1.65 g, 6.5 mmol) and imidazole (0.485 g, 7.12 mmol) then stirring is continued at 0° C. for 45 min. To this is added (S)-2-tert-butoxycarbonylamino-3-hydroxypropionic acid tert-butyl ester (0.81 g, 3.1 mmol) and the suspension is refluxed for 45 min. The suspension is filtered and the organic layer is washed with a saturated sodium bisulfite solution, water and brine, and dried over sodium sulfate. The solvent is removed under reduced pressure to afford the title compound as a white solid.

WORKUP

后处理

  1. temperaturethe suspension is refluxed for 45 min
  2. filtrationThe suspension is filtered
  3. washthe organic layer is washed with a saturated sodium bisulfite solution, water and brine
  4. dry with materialdried over sodium sulfate
  5. customThe solvent is removed under reduced pressure