HRID477283
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 131 mg of N-[2-(2-chloro-3-oxobutylthio)ethyl]-N'-cyano-N"-methylguanidine, 320 mg of ammonium formate, 0.6 ml of methyl orthoformate and 209 mg of sodium ammonium hydrogenphosphate tetrahydrate were added 2.5 ml of formamide and 2.5 ml of chloroform, and the mixture was refluxed for 2 hours. Then, 420 mg of sodium hydrogencarbonate was added to the mixture and the solvent was removed under reduced pressure, and the obtained residue was refined by silica gel column chromatography (developing solvent: ethyl acetate/methanol=10/1) to obtain 28 mg of a colorless oily product (the yield was 21%).
WORKUP
后处理
- temperaturethe mixture was refluxed for 2 hours
- customthe solvent was removed under reduced pressure