HRID19753

反应详情

EQUATION

反应方程式

HRID 19753 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationAfter 8 hours the solid state was filtered
  2. customthe filtrate was evaporated
  3. dissolutionThis residue was dissolved in ethyl acetate
  4. extractionthe product was extracted by addition of HCl solution (pH=1) to water
  5. additionby addition of 2N NaOH solution to pH=11
  6. extractionextracted with ethyl acetate
  7. customThe organic phase was evaporated
  8. customthe further purification