HRID747274

反应详情

EQUATION

反应方程式

HRID 747274 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(Benzhydrylidene-amino)-3-quinolin-5-yl-butyronitrile (8.36 g, 22.3 mmol) in dioxane (90 mL) was hydrolyzed with 1M HCl (90 mL) and the solution was stirred at rt for 16 h. The dioxane was removed under vacuum and the mixture was made basic with 2 M NaOH. The aqueous solution was extracted with chloroform:isopropanol (3:1). The organic extracts were pooled, dried over MgSO4, filtered and evaporated to leave an oil. The oily residue was purified by chromatography on SiO2, eluting with ethyl acetate and 5% methanol:ethyl acetate to give 2-amino-3-quinolin-5-yl-butyronitrile (Intermediate-E2) as a yellow solid 3.61 g (77%).

WORKUP

后处理

  1. customThe dioxane was removed under vacuum
  2. extractionThe aqueous solution was extracted with chloroform:isopropanol (3:1)
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. customevaporated
  6. customto leave an oil
  7. customThe oily residue was purified by chromatography on SiO2
  8. washeluting with ethyl acetate and 5% methanol