In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 711-01-3, name is Methyl adamantane-1-carboxylate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C12H18O2
To 40 g (206 mmol) of methyl 1-adamantanecarboxylate obtained in Production Example 1, 40 g of toluene was added and the atmosphere was replaced with nitrogen, and cooled with refrigerant. While keeping the toluene solution at 10 ° C. or less, 247 g (494 mmol) of methyl magnesium chloride in THF solution (2 M) was added dropwise over 4.5 hours. After that, the temperature was raised naturally and the reaction was carried out at room temperature (25 ° C.) for 3 hours. The reaction solution was again cooled with a coolant, while keeping the temperature below 10°C, 82.3 g (534 mmol) of methacrylic anhydride was added dropwise over 3.3 hours. Thereafter, the temperature was allowed to rise naturally, and the reaction was allowed to proceed at room temperature (25 ° C.) for 3 hours. The measurement results of this crude reaction solution by GC were as follows. Residual material = methyl 1-adamantanecarboxylate: 1.5percent, By-product = 1-(1-adamantyl) -1-methylethanol: 7.3percent and target product=1- (1-adamantyl) -1-methylethyl methacrylate: 91.2percent. While maintaining the crude reaction solution at 25 ° C. or less, magnesium salt was decomposed with hydrochloric acid aqueous solution, the aqueous layer was separated. After washing with 10percent aqueous sodium hydroxide solution and saturated brine, and concentrated. By concentrating the concentrated solution from methanol, 1-(1-adamantyl)-1-methylethyl methacrylate (37 g) was obtained. The isolation yield was 68.5percent. The purity measured by GC was 98.3percent by mass.
The synthetic route of 711-01-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Osaka Organic Chemical Industry Co., Ltd.; Tanaka, Shinji; Uenoyama, Yoshitaka; Kono, Naoya; Ono, Hidetoshi; Kojima, Akio; (11 pag.)JP5993171; (2016); B2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics