Yield:105-16-8 94.1%

Reaction Conditions:

with 10H-phenothiazine;lithium hydroxide in hexane at 65 - 73; for 5 h;Reagent/catalyst;

Steps:

1 Example 1
(1) Synthesis: 240 g (2.4 mol) of methyl methacrylate,117 g (1.0 mol) of diethylaminoethanol, 200 g of n-hexane,8 g of lithium hydroxide and 0.5 g of phenothiazine were added with stirring,Thermometer and water separator in a 1000 mL three-necked flask,Heated to 65 ° C ~ 73 ° C, constantly reflux and separation of methanol,The reaction was stopped (about 5 h) after refluxing to the absence of methanol separation.34.5 g of methanol was separated,Gas chromatographic analysis showed that the methanol content was 88.6%The methyl methacrylate content was 11.2%.(2) purification: cooling to room temperature, add 300mL × 2 of deionized water washed twice. The oil was gradually decompressed (0 to 100 mmHg) at 60 ° C to 100 ° C,Unreacted methyl methacrylate and diethylaminoethanol,And then diethyl etherate methacrylate was distilled off under reduced pressure at 5 to 10 mmHg and 90C to 100C. The resulting product was 175.7 g (theoretical yield 185.26 g) in a yield of 94.1%.Gas chromatographic analysis showed that the content of diethylaminoethyl methacrylate was99.2%.

References:

Qingdao University of Science and Technology;Tang Linsheng;Yang Jingwei;Wu Hongzhi;Hou Xiaomin;Zhu Xin;Mi Chengjing CN106966913, 2017, A Location in patent:Paragraph 0020; 0021; 0022; 0023; 0024-0028; 0035-0043

FullText