反应 #48031

反应方程式

N,N-dimethyl-N′-phenyl-chloroformamidine hydrochloride

1-methylaminooxy-2-hydroxy-3-(1-piperidinyl)-propane

Na2CO3

→

title compound

收率 10.0%

N,N,N′-trimethyl-N′-[3-(1-piperidinyl)-propoxy]N″-phenyl-guanidine

收率 10.0%

溶剂

chloroform

chloroform

反应条件

后处理

1. 1
   过滤After 8 hours the solid state was filtered
2. 2
   其他the filtrate was evaporated
3. 3
   workup.DISSOLUTIONThis residue was dissolved in ethyl acetate
4. 4
   萃取the product was extracted by addition of HCl solution (pH=1) to water
5. 5
   workup.ADDITIONby addition of 2N NaOH solution to pH=11
6. 6
   萃取extracted with ethyl acetate
7. 7
   其他The organic phase was evaporated
8. 8
   其他the further purification

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.

来源