反应详情

温度

0 °C

To a solution of methyl 2-amino-5-bromobenzoate (3.03 mL, 17.4 mmol) in THF (28 mL) was added 2-(4-chlorophenoxy)acetyl chloride (3.92 g, 19.1 mmol) to form a suspension. An additional 30 mL of dichloromethane was added. The reaction was then cooled to 0° C. and triethylamine (5.32 mL, 38.3 mmol) was added dropwise. The cold bath was removed and the reaction was stirred at room temperature for 2 hours. Analysis showed the reaction to be incomplete, so additional 2-(4-chlorophenoxy)acetyl chloride (0.5 mL, 3.22 mmol) was added and reaction solution was stirred for 1 hour then transferred to a reparatory funnel with dichloromethane dilution. The organic phase was washed with water and saturated aqueous NH4Cl solution, then dried (MgSO4), filtered, and concentrated to yield the title compound.

1. customto form a suspension
2. customThe cold bath was removed
3. customthe reaction
4. customreaction solution
5. stirringwas stirred for 1 hour
6. washThe organic phase was washed with water and saturated aqueous NH4Cl solution
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. concentrationconcentrated