HRID1908960

反应详情

EQUATION

反应方程式

HRID 1908960 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2.90 g of triphenylphosphine and 15 mL of tetrahydrofuran were added to 100 mL flask and the resulting reaction solution was cooled to 0° C. 2.17 mL of diisopropylazodicarboxylate was dropped while the reaction solution was stirred. After 30 minutes, 10 mL of tetrahydrofuran solution with 1.52 g of (S)-t-butyl 3-(t-butoxycarbonylamino)-4-hydroxybutanoate was dropped and stirred for 16 hours while the reaction temperature was naturally increased to room temperature. After completing the reaction, 40 mL of ethyl acetate and 40 mL of water were added to the reaction solution and then stirred for 10 minutes. An organic layer was isolated, dehydrated with magnesium sulfate, and then concentrated under reduced pressure. A concentrated residue was isolated with column chromatography (n-hexane:ethyl acetate=15:1) and then concentrated under reduced pressure to obtain 1.04 g of a title compound.

WORKUP

后处理

  1. customthe resulting reaction solution
  2. stirringstirred for 16 hours while the reaction temperature
  3. temperaturewas naturally increased to room temperature
  4. additionwere added to the reaction solution
  5. stirringstirred for 10 minutes
  6. customAn organic layer was isolated
  7. concentrationconcentrated under reduced pressure
  8. customA concentrated residue was isolated with column chromatography (n-hexane:ethyl acetate=15:1)
  9. concentrationconcentrated under reduced pressure