HRID435463

反应详情

EQUATION

反应方程式

HRID 435463 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the solution of 1.5 g of 1-(4-carbomethoxy-2-methylbutanoyl)-1,2,3,4-tetrahydroquinoline-2-carboxylic acid methyl ester in 13.5 ml of methanol is added 13.5 ml of N aqueous sodium hydroxide and the mixture is stirred at room temperature for 3 hours. It is concentrated at room temperature and reduced pressure, the aqueous solution filtered, cooled and acidified with concentrated hydrochloric acid. The mixture is extracted with methylene chloride, the extract dried, evaporated, the residue recrystallized from petroleum ether and triturated with diethyl ether, to yield the 1-(4-carboxy-2-methylbutanoyl)-1,2,3,4-tetrahydroquinoline-2-carboxylic acid melting at 117°-119°.

WORKUP

后处理

  1. concentrationIt is concentrated at room temperature
  2. filtrationreduced pressure, the aqueous solution filtered
  3. temperaturecooled
  4. extractionThe mixture is extracted with methylene chloride
  5. customthe extract dried
  6. customevaporated
  7. customthe residue recrystallized from petroleum ether
  8. customtriturated with diethyl ether