HRID1522471

反应详情

EQUATION

反应方程式

HRID 1522471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a solution of ethyl 1-(1-methylethyl)-6-propyl-1H-pyrazolo[3,4-b]pyridine-4-carboxylate (180 mg, 0.654 mmol) in ethanol (5 mL) and THF (1 mL) was added sodium hydroxide (1.090 mL, 3.27 mmol), and the mixture was stirred at 40° C. for 1 h. The volatiles were removed under reduced pressure. The aqueous phase was acidified to pH 3 with aq. 1N HCl. The solid precipitate formed was collected by filtration and dried under high vacuum to give 144 mg (89%) of product, which was used for next reaction without further purification. LCMS E-S (M+H)=248.1 1H NMR (400 MHz, DMSO-d6) δ ppm 0.82-1.12 (m, 3 H), 1.50 (d, J=6.6 Hz, 6 H), 1.78 (m, 2 H), 2.80-3.11 (m, 2 H), 5.09-5.38 (m, 1 H), 7.47-7.72 (s, 1 H), 8.18-8.46 (s, 1 H), 13.82 (s, 1 H).

WORKUP

后处理

  1. customThe volatiles were removed under reduced pressure
  2. customThe solid precipitate formed
  3. filtrationwas collected by filtration
  4. customdried under high vacuum