反应详情

Ethylmalonyl chloride (17 ml, 131 mmol) is added drop-wise to a solution of 5-chloro-2-chloroacetyl-4-methoxyaniline (17 g, 73 mmol) and triethylamine (18.5 ml, 131 mmol) in anhydrous acetonitrile (310 ml), under argon and at 0° C. Agitate for 2 h at ambient temperature, then add drop-wise at 0° C. a solution of sodium ethanolate in ethanol (obtained by 1.88 g, 80 mmol, of sodium in 90 ml of ethanol). Agitated for 12 hours at ambient temperature. Add 300 ml of water, agitate for another 20 minutes. Filter the precipitate; wash with water, ethanol, and ethyl ether. After drying in vacuum, 16.7 g of a yellowish solid is obtained.

1. customat 0° C
2. stirringAgitated for 12 hours at ambient temperature
3. stirringagitate for another 20 minutes
4. filtrationFilter the precipitate
5. washwash with water, ethanol, and ethyl ether
6. customAfter drying in vacuum