HRID574992

反应详情

EQUATION

反应方程式

HRID 574992 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A molar solution of sodium hydroxide (116 mL/0.116 mol) is added to a solution of ethyl 1-benzyl-6-chloro-1H-pyrazolo[3,4-b]pyridine-4-carboxylate (30.5 g/96.8 mmol) in 195 mL of THF. The mixture is stirred at ambient temperature for 2 hours and then run into a saturated aqueous solution of NaHCO3. The aqueous phase is washed with ethyl acetate and then acidified with a solution of KHSO4 (1 M) and extracted with EtOAc. The organic phase is dried over sodium sulphate and then concentrated to dryness. The product is taken up with diisopropyl ether, filtered, and then dried under vacuum to give 27.3 g of a pale yellow powder (yield: 98%).

WORKUP

后处理

  1. washThe aqueous phase is washed with ethyl acetate
  2. extractionextracted with EtOAc
  3. dry with materialThe organic phase is dried over sodium sulphate
  4. concentrationconcentrated to dryness
  5. filtrationfiltered
  6. customdried under vacuum