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
344 mg (2.0 mmole) 1-methylaminooxy-2-hydroxy-3-(1-piperidinyl)-propane was dissolved in chloroform and 220 mg of Na2CO3 was added, then a solution of 438 mg (2.0 mmole) of N,N-dimethyl-N′-phenyl-chloroformamidine hydrochloride in 3 ml of chloroform was added dropwise. After 8 hours the solid state was filtered and the filtrate was evaporated. This residue was dissolved in ethyl acetate and the product was extracted by addition of HCl solution (pH=1) to water. The aqueous phase was made alkaline then by addition of 2N NaOH solution to pH=11, and extracted with ethyl acetate. The organic phase was evaporated, and the further purification was made by column chromatography to give the title compound as a yellow oil.
WORKUP
后处理
- filtrationAfter 8 hours the solid state was filtered
- customthe filtrate was evaporated
- dissolutionThis residue was dissolved in ethyl acetate
- extractionthe product was extracted by addition of HCl solution (pH=1) to water
- additionby addition of 2N NaOH solution to pH=11
- extractionextracted with ethyl acetate
- customThe organic phase was evaporated
- customthe further purification