HRID977132

反应详情

EQUATION

反应方程式

HRID 977132 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-ethyl-4-chloro-1H-pyrazolo[3,4-b]quinoline (1.0 g, 4.3 mmol), DMSO (3 ml) and 4-(aminomethyl)pyridine (0.92 ml, 9 mmol) was heated at 80°-90° C. overnight. The reaction mixture was poured into water (200 ml)NH4OH (1 ml) and the mixture was extracted with CH2Cl2 (3×100 ml). The CH2Cl2 layers were combined, dried over MgSO4 and evaporated. The residue was crystallized from ethyl acetate and recrystallized from ethyl acetate to afford 450 mg of 1-ethyl-N-(4-pyridinylmethyl)-1H-pyrazolo[3,4-b]quinolin-4-amine, m.p. 191°-192° C.

WORKUP

后处理

  1. temperaturewas heated at 80°-90° C. overnight
  2. extractionthe mixture was extracted with CH2Cl2 (3×100 ml)
  3. dry with materialdried over MgSO4
  4. customevaporated
  5. customThe residue was crystallized from ethyl acetate
  6. customrecrystallized from ethyl acetate