HRID1494532

反应详情

EQUATION

反应方程式

HRID 1494532 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of N-(1-benzylpiperid-4-yl)-2-acetoxy-4-acetamido-5-nitrobenzamide (4.5 g; 0.01 mol) [prepared by the procedure described in Example 1] in ethanol (25 ml), concentrated hydrochloric acid (4.5 ml) and water (50 ml) was boiled under reflux for 2 hours. The mixture was diluted with water, made alkaline with sodium bicarbonate and extracted with chloroform. The organic solution was dried (Na2SO4), the solvent removed in vacuo and the residue triturated with diethyl ether to give a solid which was treated with a saturated solution of hydrogen chloride in ethanol. After crystallization from ethanol, 3 g of N-(1-benzylpiperid-4-yl)-2-hydroxy-4-amino-5-nitrobenzamide hydrochloride were obtained, m.p. 248°-250° C. (dec).

WORKUP

后处理

  1. customprepared by the procedure
  2. temperatureunder reflux for 2 hours
  3. extractionextracted with chloroform
  4. dry with materialThe organic solution was dried (Na2SO4)
  5. customthe solvent removed in vacuo
  6. customthe residue triturated with diethyl ether
  7. customto give a solid which
  8. customAfter crystallization from ethanol