As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 2568-33-4, name is 3-Methylbutane-1,3-diol, molecular formula is C5H12O2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. Quality Control of 3-Methylbutane-1,3-diol
Into a 1 L three-necked flask equipped with a stirrer, a dry air inlet tube, a thermometer, a distillation column (inner diameter 25 mm × height 300 mm, packing tower packed with 6 mm McMahon packing) and a distillation head,100 g of 3-methyl-3-hydroxy-1-butyl alcohol, 5.1 g of Zn-acetylacetonate and 33 g of hexane as a catalyst, and the inside of the system was heated to 100 to 110 C. with stirring. 15 g of hexane was withdrawn from the top of the distillation column.After cooling the inside of the system to 40 C., 240 g of methyl methacrylate and 0.24 g of 2,2,6,6-tetramethyl-4-hydroxypiperidine-N-oxide as a polymerization inhibitor were charged and stirred while blowing in a small amount of air While heating the inside of the system to 100 to 130 C. Methanol produced as the reaction proceeds proceeds by azeotropic distillation with methyl methacrylate,The reaction was gradually withdrawn from the top of the distillation column to proceed the reaction.The conversion rate of 3-methyl-3-hydroxy-1-butyl alcohol after 7 hours from the start of the reaction was 97.5%3-methyl-3-hydroxy-1-butyl alcoholThe yield of 3-methyl-3-hydroxy-1-butyl methacrylate was 77.0%, and the diester yield based on 3-methyl-3-hydroxy-1-butyl alcohol was 10.8%
With the rapid development of chemical substances, we look forward to future research findings about 2568-33-4.
Reference:
Patent; Mitsubishi Gas Chemical Company; Kushida, Eriko; Takemoto, Makiko; (16 pag.)JP2018/135285; (2018); A;,
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