1-(2,6-DIMETHYLPHENYL)-5-OXOPYRROLIDINE-3-CARBOXYLIC ACID synthesis

Yield:63674-48-6 70%

Reaction Conditions:

at 130; for 0.75 h;

Steps:

1.a

Example 1: Synthesis of l-(2,6-dimethyIphenyl)-3-isopropyl-5-oxo-pyrrolidine-3- carboxylic acid [3,5-bis(trifluoromethyl)phenyl] amidestep e step d[0072] a) A mixture of 2,6-dimethylaniline (121 g, 1 mol) and itaconic acid (130 g, 1 mol) was heated to 130 °C for 45 min in a flask open to the atmosphere, letting the generated steam vent. The heating source was removed and 0.8 L of ethyl acetate was added under vigorous stirring, while the mixture was still hot (allowing initially for some reflux). The mixture was then let to cool to room temperature while stirring. The solids were filtered off, washed with 0.4 L of ethyl acetate and dried in air to give 164 g (70% yield) of colorless crystals. LC-MS R_t (retention time): 0.54 min, MS: (ES) mlz 234 (M+H⁺).

References:

WO2011/35332,2011,A1 Location in patent:Page/Page column 25-26