2-Methylene-1,3-dioxepane synthesis
- 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%.
54237-96-6
1 suppliers
inquiry
5337-72-4
61 suppliers
$44.00/25mL
69814-56-8
80 suppliers
$70.00/100mg
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
![2-BROMOMETHYL-[1,3]DIOXEPANE](/StructureFile/ChemBookStructure3/GIF/CB4290553.gif)
57626-95-6
10 suppliers
inquiry
69814-56-8
80 suppliers
$70.00/100mg
54237-96-6
1 suppliers
inquiry
69814-56-8
80 suppliers
$70.00/100mg
75-85-4
357 suppliers
$9.00/10ml
54237-96-6
1 suppliers
inquiry
1634-04-4
693 suppliers
$14.00/100g
107-21-1
1378 suppliers
$10.00/25g
69814-56-8
80 suppliers
$70.00/100mg