ChemicalBook CAS DataBase List 2-Methylene-1,3-dioxepane

2-Methylene-1,3-dioxepane synthesis

8synthesis methods

Product Name:2-Methylene-1,3-dioxepane
CAS Number:69814-56-8
Molecular formula:C6H10O2
Molecular Weight:114.14

54237-96-6

78-92-2

69814-56-8

General procedure for the synthesis of 2-methylene-1,3-dioxane from 2-chloromethyl-1,3-dioxane (cas:54237-96-6) and sec-butanol: In a four-necked, 1-liter round-bottomed flask fitted with a thermometer, a reflux condenser, a pressurized dosing funnel, and a mechanical stirrer, 62.5 g of potassium hydroxide and 47 g of sec-butanol were added. The mixture was heated to 125 °C until all potassium hydroxide particles were completely dissolved. Subsequently, 37.5 g of 2-chloromethyl-1,3-dioxane synthesized according to the method of Example 1 was slowly added dropwise through the addition funnel. After the dropwise addition was completed, the reaction was continued for 2 hours. After completion of the reaction, the heating was stopped and 100 g of distilled water and 50 g of toluene were added to the reaction mixture. The mixture was transferred to a separatory funnel and the organic phase was separated. A sample of the reaction mixture was analyzed by gas chromatography to confirm that 2-chloromethylidene-1,3-dioxepane was completely converted and that the crude yield of 2-methylidene-1,3-dioxepane was 72%.

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Yield:69814-56-8 97.4%

Steps:

14 EXAMPLE 14

EXAMPLE 14 The procedure was as in Example 12, except that 32.0 g (0.25 mol) of 2,6-dimethylcyclohexanol were used instead of the 3,3-dimethylbutan-2-ol. The conversion of 2-chloromethyl-1,3-dioxepane was 97.4% and the yield of 2-methylene-1,3-dioxepane was 87.9%.

References:

US5455361,1995,A