HRID1702592

反应详情

EQUATION

反应方程式

HRID 1702592 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 23.6 g. (0.06 mol) methyl 2-[3-(4-benzamidopiperidino)-propoxy]-benzoate (see Example 2a), 200 ml. ethanol and 200 ml. 1 N aqueous sodium hydroxide solution is heated under reflux for 1 hour, then evaporated and the evaporation residue dissolved in water and acidified with dilute hydrochloric acid. This is followed by extraction with a mixture of 9 parts by volume of methylene chloride and 1 part by volume of ethanol. The extract is evaporated and the residue obtained is taken up in acetone and the hydrochloride of the desired product is precipitated out by the addition of ethereal hydrochloric acid. There are obtained 14.5 g. (59% of theory) 2-[3-(4-benzamidopiperidino)-propoxy]-benzoic acid hydrochloride; m.p. 207°-208° C.

WORKUP

后处理

  1. additionA mixture of 23.6 g
  2. temperatureunder reflux for 1 hour
  3. customevaporated
  4. dissolutionthe evaporation residue dissolved in water
  5. extractionThis is followed by extraction with a mixture of 9 parts by volume of methylene chloride and 1 part by volume of ethanol
  6. customThe extract is evaporated
  7. customthe residue obtained
  8. customthe hydrochloride of the desired product is precipitated out by the addition of ethereal hydrochloric acid
  9. customThere are obtained 14.5 g