HRID19953
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
PROCEDURE
实验过程
To a solution of OBS02015 (3.93 g, 10.10 mmol) in anhydrous-DCM (50 mL) was added thionyl chloride (1.11 mL, 15.15 mmol). The mixture was stirred at room temperature for 2 h and the volatiles removed in vacuo. The residue was re-dissolved and co-evaporated three times with DCM (3×20 mL) to give OBS02018 as a brown oil which solidified on standing (3.93 g, 96%). TLC [SiO2, EtOAc-n-hexane (1:1)] Rf=0.83; 1H-NMR (270 MHz, CDCl3)=3.11 (6H, s), 4.46 (2H, s) 7.59 (2H, s).
WORKUP
后处理
- customthe volatiles removed in vacuo
- dissolutionThe residue was re-dissolved