HRID246633

反应详情

EQUATION

反应方程式

HRID 246633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-20 °C

PROCEDURE

实验过程

6-Fluoro-3-iodo-1H-indazole (300 mg, 1.1 mmol) in 30 mL of dry THF was cooled to −20° C. under nitrogen atmosphere, then isopropylmagnesium chloride (1.2 mL, 2.42 mmol) was added and mixture stirred for 15 mins at −20° C. Tributylchlorostannane (0.4 mL, 1.32 mmol) was added and the reaction mixture was allowed to warm to room temperature and stirred for 1 h. The reaction was quenched with saturated ammonium chloride, product extracted with ethyl acetate (3×50 mL), dried with sodium sulphate, filtered and concentrated to give 6-fluoro-3-(tributylstannyl)-1H-indazole (500 mg, crude) as a colorless oil which was used directly in the next step without further purification.

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. stirringstirred for 1 h
  3. customThe reaction was quenched with saturated ammonium chloride, product
  4. extractionextracted with ethyl acetate (3×50 mL)
  5. dry with materialdried with sodium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated