HRID1173129

反应详情

EQUATION

反应方程式

HRID 1173129 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
195 °C

PROCEDURE

实验过程

p-Cymene (100 ml) and palladium carbon (0.9 g) were added to 6-ethoxycarbonylamino-1-methyl-3,4-dihydroisoquinoline, followed by heating under stirring at 195° C. for one hour in a nitrogen atmosphere. The catalyst was filtered off and washed with ethanol, and then the filtrate was partially evaporated. After extracting with 1N hydrochloric acid, the extract was basified with potassium carbonate and then extracted with ethyl acetate. The extract was washed with brine and dried over anhydrous magnesium sulfate anhydride. The solvent was evaporated, to give the title compound (0.629 g, 69%, 2 steps) as pale yellow crystals.

WORKUP

后处理

  1. temperatureby heating
  2. filtrationThe catalyst was filtered off
  3. washwashed with ethanol
  4. customthe filtrate was partially evaporated
  5. extractionAfter extracting with 1N hydrochloric acid
  6. extractionextracted with ethyl acetate
  7. washThe extract was washed with brine
  8. dry with materialdried over anhydrous magnesium sulfate anhydride
  9. customThe solvent was evaporated