HRID1452837

反应详情

EQUATION

反应方程式

HRID 1452837 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

N-(3-Fluorophenyl)-(1H-indazol-5-yl)sulfonamide can be obtained in the following way: 0.98 ml of 3-fluoroaniline is added dropwise to a solution, cooled to a temperature in the region of 0° C., of 2.57 g of (1H-indazol-5-yl)sulfonyl chloride in 40 ml of pyridine. Stirring is maintained for 2 hours at a temperature in the region of 0° C. and then for 18 hours at a temperature in the region of 20° C. The medium is concentrated by evaporation under reduced pressure, and the residue obtained is taken up with 50 ml of ethyl acetate and 40 ml of water. The organic phase is washed with 2 times 20 ml of water, dried over magnesium sulfate, filtered and concentrated by evaporation under reduced pressure. The residue obtained is purified by chromatography on a silica column with an ethyl acetate/cyclohexane (1/3 by volume) mixture as eluent. 8 mg of N-(3-fluorophenyl)-(1H-indazol-5-yl)sulfonamide are thus obtained in the form of an orange solid.

WORKUP

后处理

  1. concentrationThe medium is concentrated by evaporation under reduced pressure
  2. customthe residue obtained
  3. washThe organic phase is washed with 2 times 20 ml of water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated by evaporation under reduced pressure
  7. customThe residue obtained
  8. customis purified by chromatography on a silica column with an ethyl acetate/cyclohexane (1/3 by volume) mixture as eluent