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ChemicalBook CAS DataBase List ETHYL 5-NITROBENZOFURAN-2-CARBOXYLATE
69604-00-8

ETHYL 5-NITROBENZOFURAN-2-CARBOXYLATE synthesis

8synthesis methods
-

Yield: 95.2%

Reaction Conditions:

with potassium carbonate in N,N-dimethyl-formamide at 85 - 90; for 15 h;Inert atmosphere;

Steps:

1 Example-1: Preparation of ethyl 5-nitro-l-benzofuran-2-carboxylate
Example-1: Preparation of ethyl 5-nitro-l-benzofuran-2-carboxylate To a solution of DMF (400ml), K2C03 powder (124. lg) and 5-nitro salicylaldehyde (lOOg) was slowly added Diethyl bromomalonate (171.7g) at 30-40°C under Nitrogen atmosphere. The reaction mixture was stirred at 85-90°C under Nitrogen atmosphere for 15 hours. Cool the reaction mix to 80-85°C. Cyclohexane (500ml) was added to the reaction mix at 70-85°C within 1 hour and then stirred the reaction mix at 80-85°C for 15-30 minutes. The reaction mixture was cooled to 15-20°C and process water (1000ml) was added to the reaction mixture at 15-20°C within 1 hour. The reaction mixture was stirred at 20-30°C for 1-2 hour and then the solid was filtered and washed with process water (100mlx5). Dried at 55-60°C. for 8-10 hours. Yield: 95.2%

References:

ALEMBIC PHARMACEUTICALS LIMITED;JAYARAMAN, Venkat Raman;RATHOD, Dhiraj;VOHRA, Irfan;BHUJADE, Vinayak;MODI, Viral;GANDHI, Ojas;BUDH, Mayur WO2013/153492, 2013, A2 Location in patent:Page/Page column 23