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ChemicalBook CAS DataBase List 4-Fluoro-N-isopropylbenzamide

4-Fluoro-N-isopropylbenzamide synthesis

2synthesis methods
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Yield:70001-45-5 95%

Reaction Conditions:

Stage #1: 4-Fluorobenzoic acidwith thionyl chloride in dichloromethane;Reflux;
Stage #2: diisopropylaminewith triethylamine in dichloromethane at 20;Solvent;

Steps:

1.1.1; 1.1.2 Synthesis of compound III

1.1 Add 140g of compound II, 14g of DMF, 700ml of dichloromethane to a 2L three-necked reaction flask, stir to dissolve, cool down in a water bath, control the temperature below 30 °C, add 238g of thionyl chloride, 1-2 hours after dropping. The system was heated to reflux, reacted for 3-5 hours, concentrated to dryness, added 300ml of dichloromethane, stirred and dissolved. The temperature is controlled at 10-30 °C and the mixed system composed of 150g of triethylamine and 132g of diisopropylamine is added dropwise, dripping in 1-2 hours, and reacting at room temperature for 5-8 hours. After the reaction is completed, water is added to wash, the organic phase is concentrated to dryness, be slurried with petroleum ether, filtered, and dried to obtain 211 g of off-white product with a yield of 95%.

References:

CN112724077,2021,A Location in patent:Paragraph 0028; 0029