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ChemicalBook CAS DataBase List Mecarbinate
15574-49-9

Mecarbinate synthesis

11synthesis methods
Ethyl 3-(methylamino)-2-butenoate

870-85-9

1,4-Benzoquinone

106-51-4

Mecarbinate

15574-49-9

Synthesis: To a 250 ml round bottom flask was added p-benzoquinone (11.89 g, 0.11 mol) and 120 ml acetone and stirred well. Subsequently, a solution containing 0.11 mol of ethyl 3-(methylamino)-2-butenoate was added slowly and dropwise. The reaction mixture was stirred at 30°C for 2 hours. After completion of the reaction, the solvent was removed by distillation. The crude product was purified by recrystallization using acetone.

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Yield:15574-49-9 74.9%

Reaction Conditions:

in 1,2-dichloro-ethane at 50; for 12 h;Reflux;

Steps:

1.2 Step 2: Synthesis of Intermediate 3
P-benzoquinone (9.1 g, 83.81 mmol) was dissolved in 1,2-dichloroethane and heated to 50 ° C.Then a solution of Intermediate 2 (10.0 g, 69.84 mmol) in 1,2-dichloroethane was slowly added dropwise.After the completion of the dropwise addition, the reflux reaction was continued for 12 hours, and the reaction was completed by TLC, and the solid was washed off by cooling.Filtration was carried out to obtain 12.2 g of Intermediate 3 in a yield of 74.9%.

References:

Henan University;Wang Honggang;Wu Dongdong;Ge Zhenying;Chen Mingliang;Lv Shuangyu;Nie Xiaobo;Liu Fengtao;Wang Yizhen CN110092791, 2019, A Location in patent:Paragraph 0019; 0039; 0043-0044

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