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. 39495-82-4, name is Ethyl 5-methylhex-5-enoate, A new synthetic method of this compound is introduced below., Quality Control of Ethyl 5-methylhex-5-enoate
A 100-mL RBF with magnetic stirrer,was flame-dried under vacuum and back-filled with a nitrogen atmosphere, then chargedwith Ethyl 5-methyl-5-hexenoate (1.5 g, 9.60 mmol) and dry DCM (30 mL). The solutionwas cooled to -78 C before the dropwise addition of diisobutylaluminium hydride (10.37mL, 1.01 M in hexanes). The mixture was stirred at this temperature for 1 h, then excessDIBAL-H was quenched by the addition of 1.0 M HCl (aq) (10 mL). Dichloromethane(30 mL) was added and the solution was warmed to 23 C and the biphasic mixture wasseparated. The Organic layer was washed with 1.0 M HCl (aq) (15 mL), the aqueouslayers were combined and extracted with DCM (2 x 15 mL). All organic layers were combined and pushed through a plug of Celite, washing with DCM (2 x 10 mL). TheDCM solution containing 5-methylhex-5-enal was transferred to a 250-mL RBF,equipped with a magnetic stirrer and dried with MgSO4 before the addition of N,Ndimethylhydrazine(1.15 g, 19.2 mmol). This mixture was stirred for 4 h at 23 C, filtered,concentrated in vacuo and purified by vacuum transfer distillation (0.5 torr) to yield 1.22g of the title compound as a colorless oil.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Article; Mickelsen, Ky; Zabawa, Sean; Livinghouse, Tom; Synlett; vol. 29; 2; (2018); p. 181 – 184;,
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