3-Methyl-3-oxetanemethanol synthesis
- Product Name:3-Methyl-3-oxetanemethanol
- CAS Number:3143-02-0
- Molecular formula:C5H10O2
- Molecular Weight:102.13
77-85-0
3143-02-0
In a three-necked flask equipped with a stirrer, a reflux condenser and a thermometer, 215 mL of diethyl carbonate, 180 g of trimethylolpropane, and an appropriate amount of KOH were added.The mixture was heated with stirring to 115° C. and kept at reflux for 1 hr. The by-product alcohol was collected via a reflux distillation unit. Continued heating of the reaction mixture and subsequent distillation to collect the 205-210 °C fractions afforded the target product 3-hydroxymethyl-3-methoxybutane (2) in a total amount of 128.2 g in 83.7% yield. The structure of the product was confirmed by 1HNMR (Figure 2).
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3143-02-0
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Yield:3143-02-0 83.7%
Reaction Conditions:
with potassium hydroxide;Diethyl carbonate at 115; for 1 h;
Steps:
1.1 1,Synthetic route for preparing the compound (2) 3-methyl-3-hydroxymethyl oxetane
Equipped with a stirrer, a reflux condenser and a thermometer three-necked flask, followed by adding diethyl carbonate 215ml, trimethylolethane 180g and Κ0Η0. Lg. Heated under stirring to 115 ° C, the reaction was refluxed for lh, the means to reflux distillation apparatus, collecting by-product alcohol was distilled, heating was continued and then distilled collecting the fraction 205~210 ° C to give product 3-hydroxymethyl-3 - methyl-oxetane (2) total 128. 2g. The yield was 83.7%. Its 1HNMR see Figure 2.
References:
CN103772347,2016,B Location in patent:Paragraph 0019; 0020; 0021
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