Ethyl-2-(diphenylaMino)pyriMidine-5-carboxylate synthesis

Yield:1316216-05-3 69.9%

Reaction Conditions:

with copper (I) iodide;Cs₂CO₃ in N,N-dimethyl-formamide at 140; for 12 h;Inert atmosphere;

Steps:

1-2 Synthesis of Intermediate 3:

In a 500ml three-necked flask, add compound 2 (17.00g, 70mmol),Iodobenzene (17.11g, 84mmol), cesium carbonate (45.54g, 140mmol),Cuprous iodide (6.65g, 35mmol), DMF 200ml, under nitrogen protection at 140 for 12h.Cool to room temperature, add 200 ml of ethyl acetate to dilute, filter to remove copper salt, add 200 ml of water to the filtrate, stir at room temperature for 20 min, separate the liquid, and extract the aqueous phase twice with 100 ml of ethyl acetate.Combine the organic phases, add 200ml of EDTA saturated solution, stir for 30min, and separate the organic layer.Wash with 100ml of saturated saline, concentrate to dryness under reduced pressureObtained brown oil, recrystallized by adding 50ml of ethanol,15.6g light yellow solid was obtained,The yield was 69.90%.

References:

CN110885316,2020,A Location in patent:Paragraph 0095; 0102-0104; 0127-0130