HRID1827954

反应详情

EQUATION

反应方程式

HRID 1827954 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Isopropyl-1H-pyrazole-3-carboxylic acid (WO 03/035065, page. 485, example 17b) (1.00 g, 6.49 mmol) was dissolved in a mixture of concentrated sulphuric acid (1.5 mL) and ethanol (25 mL) and the reaction mixture heated at reflux for 3 hours. The reaction mixture was cooled, poured into water, basified with 0.88 ammonia then extracted with ethyl acetate. The ethyl acetate was washed with brine, dried over magnesium sulphate and concentrated in vacuo to yield the title product, 514 mg (43%).

WORKUP

后处理

  1. temperaturethe reaction mixture heated
  2. temperatureat reflux for 3 hours
  3. temperatureThe reaction mixture was cooled
  4. extractionthen extracted with ethyl acetate
  5. washThe ethyl acetate was washed with brine
  6. dry with materialdried over magnesium sulphate
  7. concentrationconcentrated in vacuo