2-N-Morpholinoethyl methacrylate synthesis

Yield:2997-88-8 86%

Reaction Conditions:

with potassium phosphate;4-methoxy-phenol at 70; under 225.023 Torr;

Steps:

5 Example 4Transesterification was carried out in the apparatus described in Example 1

n this apparatus, 0.28 g (350 ppm) of hydroquinone monomethyl ether, 600 g (6.0 mol) of methyl methacrylate (MMA) and 193.8 g (1.5 mol) of hydroxyethyl piperidine and 6.37 g (6.37 g) of anhydrous potassium phosphate 2.0 mol% based on hydroxyethylpiperidine) was charged and stirred. Adjusted to vacuum (300 mbar) and the suspension was slowly heated to 70 ° C. The distillate (MMA / methanol) was continuously removed during the reaction and returned according to the reflux ratio. The temperature in the bottom of the column was 70-76 ° C and the temperature at the top of the column was 38-66 ° C. The reaction was followed using GC analysis.After 270 minutes, the bath temperature was lowered to 60 ° C. and unreacted MMA was distilled off. The reaction was terminated and the vacuum was turned off. The suspension was cooled and the remaining catalyst was subsequently filtered off with pressure nutsche.A clear solution was obtained with> 99% yield of piperidinyl ethyl methacrylate having a purity of about 90%. The solution still contained 5% alcohol.The remaining alcohol was separated from the product by distillation (0.1 mbar, bottom temperature 86 ° C.).The final product was obtained in 86% yield and> 98% purity.

References:

JP5882334,2016,B2 Location in patent:Paragraph 0095-0099