HRID731710

反应详情

EQUATION

反应方程式

HRID 731710 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
142 °C

PROCEDURE

实验过程

1-(2-(4-fluorophenyl)-6-(trifluoromethyl)pyrazolo[1,5-a]pyridin-3-yl)-2-methylprop-1-enyl isobutyrate. To 2.50 g (8.9 mmol) of 2-(4-fluorophenyl)-6-(trifluoromethyl)pyrazolo[1,5-a]pyridine in 43 ml of isobutyric anhydride was added conc. H2SO4 (5 drops). The mixture was stirred and heated at 142° C. overnight. The mixture was cooled to room temperature and poured into water (120 ml) at 0° C. The solution was then adjusted to pH 10 with 2N NaOH. The aqueous layer was extracted with Et2O (3×100 ml), dried over MgSO4, filtered and concentrated. The crude product was purified by flash column chromatography (3% EtOAc-hexane) to afford 2.54 g (68%) of the title compound) as an orange solid. Compound 1033.

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. extractionThe aqueous layer was extracted with Et2O (3×100 ml)
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe crude product was purified by flash column chromatography (3% EtOAc-hexane)