Yield:-

Reaction Conditions:

with 4,4'-butylidenebis(6-tert-butyl-m-cresol) in ethylene glycol at 150; under 52.5053 Torr; for 4 h;Inert atmosphere;

Steps:

17 Example 3
General procedure: 435.2 g (3.0 mol) of N, N-diethylaminopropionic acid and 263.3 g (3.6 mol) of DEA were added to a 1,000 mL pressure-resistant reaction vessel (autoclave) equipped with a stirrer and a temperature sensor,60 g of silica 60 was added and stirred at 100 ° C. for 24 hours.After completion of the reaction,The temperature of the reaction solution was returned to room temperature,A packed tower,The reaction solution was transferred to a four-necked flask equipped with a condenser and a distillation receiver,0.6 g of TDA was added as a polymerization inhibitor.after that,As in Example 1, the pot temperature was 130 ° C.,Under the condition of a degree of vacuum of 7.0 kPa,The thermal decomposition reaction was carried out for 3 hours,378 g of crude "DEAA" (purity = 96%) was obtained.further,The obtained crude "DEAA" was purified by distillation in the same manner as in Example 1,345 g (purity 99.7%, total yield = 90%) of a high purity product "DEAA" was obtained as a colorless liquid (Table 2).

References:

KJ CHEMICALS CORPORATION;FURUSHO, HARUKA;HIRATA, MEIRI;MASUDA, HIDEKI JP2015/209419, 2015, A Location in patent:Paragraph 0055; 0061; 0062