반응 #717601

반응 방정식

Water

methanol

methyl 4-amino-5-iodo-2-methoxybenzoate

intermediate 128

methyl 4-amino-5-iodo-2-methoxybenzoate

dicyanozinc

→

title compound

수율 76.0%

methyl 4-amino-5-cyano-2-methoxybenzoate

수율 76.0%

용매

ether

dimethylformamide

반응 조건

후처리

1. 1
   추출the crude was extracted with ethyl acetate
2. 2
   세척the organic layer was washed with brine
3. 3
   기타dried
4. 4
   기타the solvent was removed under reduced pressure
5. 5
   기타The crude obtained

실험 절차

A solution of methyl 4-amino-5-iodo-2-methoxybenzoate (intermediate 128; 5 g, 16.28 mmol) and dicyanozinc (1.5 g, 12.77 mmol) in dimethylformamide (50 mL) in a slenck vessel was degasified with nitrogen. Then tetrakis (1 g, 0.87 mmol) was added and the reaction mixture was stirred at 80° C. for 2 hours. Water was added into the reaction mixture and the crude was extracted with ethyl acetate, the organic layer was washed with brine, dried and the solvent was removed under reduced pressure. The crude obtained was treated with methanol and ether to obtain the title compound as a yellow solid (76%).

출처