HRID509456

反应详情

EQUATION

反应方程式

HRID 509456 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 3-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)-5,6-dihydrobenzo[d]isoxazol-7(4H)-one (880 mg, 2.72 mmol) in THF (15 ml) at 0° C., was added slowly (3,5-difluorophenyl)magnesium bromide (6.54 mL of 0.5 M solution in THF, 3.27 mmol) and the reaction was stirred for 3 hr. Additional amount of (3,5-difluorophenyl)magnesium bromide (6.0 mL of 0.5 M solution in THF, 3.0 mmol) was added and stirring was continued at 0° C. for 2 hr. The reaction mixture was quenched with water, extracted with ethyl acetate, and the organic phase was washed with water and brine, dried over sodium sulfate and concentrated. The crude product was purified by silica gel chromatography using 0-6% MeOH in DCM as solvent to afford the 828 mg of the title product.

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued at 0° C. for 2 hr
  3. customThe reaction mixture was quenched with water
  4. extractionextracted with ethyl acetate
  5. washthe organic phase was washed with water and brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated
  8. customThe crude product was purified by silica gel chromatography