HRID477274
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
- 0 °C
PROCEDURE
实验过程
In 1 ml of methanol was dissolved 131 mg of N-[2-(2-chloro-3-oxobutylthio)]ethyl-N'-cyano-N"-methyl-guanidine, and the solution was cooled with water and 55 mg of t-butyl hypochlorite was added to the solution. The mixture was stirred at 0° C. for 1 hour and 1 ml of water and 15 ml of ethyl acetate were added to the reaction mixture. The ethyl acetate layer was recovered, dried with anhydrous sodium sulfate and concentrated under reduced pressure. The obtained residue was refined by silica gel column chromatography (developing solvent: ethyl acetate/ethanol=10/1) to obtain 24 mg of a colorless oily product (the yield was 16%).
WORKUP
后处理
- additionwas added to the solution
- customThe ethyl acetate layer was recovered
- dry with materialdried with anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure