HRID1478555
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
(S)-tert-butyl 2-((tosyloxy)methyl)morpholine-4-carboxylate (63.7 g, 171.52 mmol) was dissolved in DMF (550 ml), and then NaN3 (44.59 g, 686.08 mmol) and NaI (2.5 g, 17.15 mmol) were added, followed by stirring at 70° C. overnight. After the completion of the reaction, the reaction mixture was extracted with H2O and EA, followed by drying (Na2SO4), filtration, and concentration under reduced pressure, and the residue was purified by column chromatography (EA:Hex=1:5), to give (S)-tert-butyl 2-(azidomethyl)morpholine-4-carboxylate as a white solid (31.1 g, 75%).
WORKUP
后处理
- customAfter the completion of the reaction
- extractionthe reaction mixture was extracted with H2O and EA
- customby drying
- filtration(Na2SO4), filtration, and concentration under reduced pressure
- customthe residue was purified by column chromatography (EA:Hex=1:5)