HRID1773335

反应详情

EQUATION

反应方程式

HRID 1773335 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

AlCl3 (0.733 g, 5.50 mmol) is added to a solution of 7-(4-methoxybenzyl)-5-methyl-3-(phenylamino)-2-(4-(pyridin-2-yl)benzyl)-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione (1.08 g, 1.98 mmol) and anisole (mL) in 1,2-dichloroethane (15 mL) under argon. The reaction mixture is stirred at room temperature overnight, and then quenched with water with cooling. The resulting suspension is treated with 20% NaOH (70 mL), and then extract with methylene chloride 5 times. The organic phase is combined and evaporated to dryness. The residue is further purified by chromatography to give 751 mg of pure product (Yield: 89%). MS (FAB) m/z 425.3 [M+H]+.

WORKUP

后处理

  1. customquenched with water
  2. temperaturewith cooling
  3. additionThe resulting suspension is treated with 20% NaOH (70 mL)
  4. extractionextract with methylene chloride 5 times
  5. customevaporated to dryness
  6. customThe residue is further purified by chromatography