Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 40637-56-7, name is Dimethyl 2-allylmalonate, A new synthetic method of this compound is introduced below., COA of Formula: C8H12O4
4.1.1 2-Allyl-2-methoxycarbonyl-malonic acid dimethyl ester (5) 13 At 0 C, to a suspension of NaH (60% in mineral oil) (5.85 g, 146.2 mmol, 1.5 equiv) in THF (150 mL), was added 4 (16.78 g, 97.4 mmol) and the mixture was warmed to rt and stirred during 1 h. Then, freshly distilled ClCO2Me (20 mL, 258.0 mmol, 2.6 equiv) was slowly added at 0 C and the solution was warmed to rt and stirred during 2 h. The reaction mixture was diluted in diethyl ether and washed with saturated aqueous solution of ammonium chloride and brine, dried over MgSO4, filtered, and concentrated. Pure compound 5 (20.41 g, 88.6 mmol, 91%) was obtained as a colorless oil. 1H NMR (CDCl3, 200 MHz) delta 5.95-5.77 (ddt, J=17.2; 10.3 and 7.4 Hz, 1H, H2C=CHCH2); 5.09 (dd, J=17.2 and 1 Hz, 1H, HC=CHtrans); 4.99 (dd; J=10.3 and 1 Hz, 1H, HC=CHcis); 3.70 (s, 9H, CO2CH3); 2.78 (d, J=7.4 Hz, 2H, H2C=CHCH2). 13C NMR (CDCl3, 50 MHz) delta 166.9 (CO2CH3); 132.4 (H2C=CHCH2); 119.4 (H2C=CHCH2); 65.7 (C(CO2CH3)3); 53.1 (CO2CH3); 37.6 (H2C=CHCH2). IR (neat), cm-1: 2900; 1740; 1460; 1370; 1230. Anal. for C10H14O6 (M=230.22 g mol-1): calcd (%) : C=52.17; H=6.13. found (%) : C=52.06; H=6.32.
The synthetic route of 40637-56-7 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Agarwal, Jyoti; Commandeur, Claude; Malacria, Max; Thorimbert, Serge; Tetrahedron; vol. 69; 45; (2013); p. 9398 – 9405;,
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