1-Propanone, 1-(3,5-dimethyl-2-furanyl)- synthesis

Yield:75426-42-5 41%

Reaction Conditions:

with phosphoric acid in water at 60; for 2 h;

Steps:

2.1

Example 2.; 2-Ethyl-4,6-dimethyl-3-hydroxypyridine, succinic acid salt (1:1).; (1) 2-Propionyl-3,5-dimethylfuran; 85% Phosphoric acid (0.05 mole) is slowly dropped into a mixture of 2,4- dimethylfuran (0.3 mole, CAS registry number [3710-43-8]) and propionic anhydride (78.1 g, 0.6 mole) heated to 40⁰C. The reaction mixture is heated to 6O⁰C for 2 hours. Temperature is allowed to reach the room's one, then 120 ml of water are added, stirring for 1 more hour. The organic phase is separated and treated with sodium carbonate saturated solution, stirring for 24 hours, to destroy the untreated anhydride and acid. After that, the solution is extracted with chloroform (300 ml x 3), then the combined organic phases are dried with Na₂SO₄ and evaporated to obtain an oily residue which is distilled under vacuum, recovering the fraction boiling at 71-75°C (0.6 mm). The pure ketone is obtained (19.6 g, 41%)

References:

WO2009/78746,2009,A1 Location in patent:Page/Page column 9