HRID1528544

反应详情

EQUATION

反应方程式

HRID 1528544 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5-bromo-N,N-dimethyl-3-(trifluoromethyl)-1H-pyrazole-1-sulfonamide (i.e. the product of Example 11, Step A) (4.50 g, 14.0 mmol) and trifluoroacetic acid (2.0 mL, 26 mmol) was stirred at 25° C. for 4 h. The reaction mixture was diluted with water (20 mL), and sodium hydroxide was added to raise the pH to 12. The solution was extracted with chloroform, dried (MgSO4), and concentrated under reduced pressure to give 2.73 g of the title compound as a yellow light oil. This compound was of sufficient purity to use in subsequent reactions.

WORKUP

后处理

  1. additionwas added
  2. temperatureto raise the pH to 12
  3. extractionThe solution was extracted with chloroform
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated under reduced pressure