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ChemicalBook CAS DataBase List 3-Methyl-3-oxetanemethanol
3143-02-0

3-Methyl-3-oxetanemethanol synthesis

5synthesis methods
1,1,1-Tris(hydroxymethyl)ethane

77-85-0

3-Methyl-3-oxetanemethanol

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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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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