HRID927920

反应详情

EQUATION

反应方程式

HRID 927920 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Concentrated sulfuric acid (5 drops) was added to a solution of methyl cis-(3aRS,9bRS)-5-acetyl-7-(2,2-dimethylpropionylamino)-1,2,3a,4,5,9b-hexahydro-furo[2,3-c]quinoline-6-carboxylate (Intermediate 30, 0.15 g) in methanol (5 mL) and the solution was stirred and heated at reflux for 48 hours. After cooling, the mixture was evaporated to low volume and the residue was dissolved in ethyl acetate and carefully washed with saturated aqueous sodium bicarbonate solution. The organic layer was filtered through a phase separator and the filtrate was evaporated to dryness to give methyl cis-(3aRS,9bRS)-5-acetyl-7-amino-1,2,3a,4,5,9b-hexahydrofuro[2,3-c]quinoline-6-carboxylate (0.09 g) as a brown gum.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 48 hours
  3. temperatureAfter cooling
  4. customthe mixture was evaporated to low volume
  5. dissolutionthe residue was dissolved in ethyl acetate
  6. washcarefully washed with saturated aqueous sodium bicarbonate solution
  7. filtrationThe organic layer was filtered through a phase separator
  8. customthe filtrate was evaporated to dryness