HRID387680

反应详情

EQUATION

反应方程式

HRID 387680 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

33 mg of methyl 7-methyl-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxylate are dissolved in 1 cm3 of dioxane at a temperature close to 20° C. 0.3 cm3 of a 1N aqueous solution of sodium hydroxide is added, then the reaction mixture is heated at a temperature close to 60° C. for 1 h. The mixture is then concentrated to dryness under reduced pressure (5 kPa), taken up by 10 cm3 of water and 15 cm3 of ethyl ether. The aqueous phase is decanted, washed with 10 cm3 of ethyl ether, acidified with 0.3 cm3 of a 2N aqueous solution of hydrochloric acid and taken up with 10 cm3 of dichloromethane. The organic phase is extracted, dried over anhydrous magnesium sulfate, filtered and concentrated to dryness under reduced pressure (5 kPa). 33.5 mg of 7-methyl-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxylic acid are obtained in the form of a colorless lacquer.

WORKUP

后处理

  1. customclose to 20° C
  2. temperaturethe reaction mixture is heated at a temperature
  3. customclose to 60° C. for 1 h
  4. concentrationThe mixture is then concentrated to dryness under reduced pressure (5 kPa)
  5. customThe aqueous phase is decanted
  6. washwashed with 10 cm3 of ethyl ether
  7. extractionThe organic phase is extracted
  8. dry with materialdried over anhydrous magnesium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated to dryness under reduced pressure (5 kPa)