phenyl hydrogen phenylmalonate synthesis

Yield:21601-78-5 86%

Reaction Conditions:

Stage #1: phenylmalonic acidwith meta-hydroxyacetanilide in toluene at 85; under 14.2514 Torr;
Stage #2: phenolwith ethylenediamine for 3.5 h;Reflux;Temperature;Pressure;Concentration;

Steps:

3 Example 3:

In a reaction vessel equipped with a stirrer and a thermometer, 0.19 mol of phenylmalonic acid and 100 ml of a 85% toluene solution were added, and 0.18 mol of N- (3-hydroxyphenyl) acetamide was slowly added thereto. 85 , the reaction time was controlled at 4-5h, 1.9kPa vacuum distillation, toluene was distilled off, the residue was added 85% ethylenediamine solution 100ml, phenol 0.17mol, heating reflux 3.5h, reduce the solution temperature to 45 , Washed with 50ml of sodium bromide solution, and then extracted with 55% potassium hydroxide solution, the pH value of the solution was controlled at 8-9, the extracts were combined and washed with 200ml of toluene solution, the water layer was 65% potassium bicarbonate Solution washing, the resulting oil-like substance with a mass fraction of 90% methylamine solution fully extracted, washed layer of methylamine, calcium oxide dehydration, steamed to the solvent, the resulting solid recrystallized from isopropanol,getcolorless39.63 g of needle-like crystalline phenylmalonic acid monophenyl ester was obtained in a yield of 86%.

References:

CN105503590,2016,A Location in patent:Paragraph 0015; 0016