HRID731736

反应详情

EQUATION

反应方程式

HRID 731736 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

1-(2-Isopropyl-pyrazolo[1,5-a]pyridin-3-yl)-2-methyl-propan-1-one (30.0 g, 115 mmole), water (100 ml), and concentrated sulfuric acid (100 ml) were combined and stirred at 130° C. for 18 hours. The mixture was cooled to room temperature and poured into a solution of ice (400 g) and water (200 ml). The solution was neutralized with sodium hydroxide solution and extracted with chloroform. The organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo. The oil was purified by vacuum distillation to give 14.9 g (81%) of 2-isopropyl-pyrazolo[1,5-a]pyridine. 1H-NMR (250 MHz, DMSO-d6) δ 8.37 (d, J=7.3 Hz, 1H), 7.41 (d, J=9.0 Hz, 1H), 7.00 (t, J=7.3 Hz, 1H), 6.66 (t, J=7.5 Hz, 1H), 6.28 (s, 1H), 3.16 (sept, J=7.0 Hz, 1H), 1.35 (d, J=6.8 Hz, 6H).

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. extractionextracted with chloroform
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. distillationThe oil was purified by vacuum distillation