HRID1968616

反应详情

EQUATION

反应方程式

HRID 1968616 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 2,4-difluorobenzoate (2 g, 11.6 mmol)), K3PO4 (2.4 g, 11.3 mmol) and 4-hydroxyindazole (1.40 g, 10.5 mmol) were stirred at 115° C. in diglyme (20 mL) for 24 hours. The reaction was cooled and poured into ether. The solution was washed three times with 1M NaOH solution, followed by brine, and then dried over Na2SO4 and filtered. The filtrate was then concentrated, and the crude product was chromatographed on silica gel with 20% ethyl acetate/hexanes.

WORKUP

后处理

  1. temperatureThe reaction was cooled
  2. washThe solution was washed three times with 1M NaOH solution
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationThe filtrate was then concentrated
  6. customthe crude product was chromatographed on silica gel with 20% ethyl acetate/hexanes