HRID2246625

反应详情

EQUATION

反应方程式

HRID 2246625 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Iodine (0.153 g) was added to a stirred solution of N-ethyl-3-fluoro-5-(1H-indazol-6-yl)-4-methylbenzamide (Intermediate 18, 0.15 g) in 1,4-dioxan (4 ml) and aqueous sodium hydroxide (2M, 4 ml) then stirred at room temperature for 45 min. The reaction mixture was treated aqueous citric acid (20%, 20 ml) followed by sodium metabisulphite (2 g). The mixture was diluted with water then extracted with ethyl acetate (2×30 ml). The organic extracts were washed with water (30 ml) dried (Na2SO4) and concentrated under vacuum to give the title-compound as a pale yellow foam (0.21 g).

WORKUP

后处理

  1. extractionthen extracted with ethyl acetate (2×30 ml)
  2. washThe organic extracts were washed with water (30 ml)
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated under vacuum