Method for synthesizing decyl acetal aldehyde
A technology for the synthesis of ten-carbon acetal and its synthesis method, which is applied in the field of synthesis of ten-carbon acetal, can solve the problems of numerous steps, high cost, and low yield, and achieve simple industrial operation, good industrialization prospects, and technical difficulty little effect
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[0025] A synthetic method of deca-acetal, comprising the following steps:
[0026] 1) The compound (E-4-acetoxy-2-methyl-2-butene-1-aldehyde) represented by the structural formula (1) is mixed with trimethyl orthoformate or triethyl orthoformate at room temperature, acidic The acetalization reaction is carried out under the action of the catalyst p-toluenesulfonic acid, and after the reaction is finished, a base is added for hydrolysis to obtain the acetal product shown in the structural formula (2),
[0027]
[0028] where R 1 is methyl or ethyl, and the molar ratio of the compound represented by the structural formula (1), trimethyl orthoformate or triethyl orthoformate, and base is 1:0.8-1.5:0.6-1.2;
[0029] 2) the acetal product obtained in the previous step and the vinyl ether compound shown in structural formula (3) are in a ratio of 1: 0.8-1.2 according to the molar ratio at room temperature, a catalyst (zinc chloride, zinc bromide, trichloride A kind of iron in i...
Example Embodiment
[0040] Example 1:
[0041] Preparation of compounds with structural formula (8)
[0042]
[0043] Get 10 grams of compounds shown in structural formula (1), add the p-toluenesulfonic acid of catalytic amount, add 10 grams of trimethyl orthoformate, react at room temperature for 10 hours, add 2 grams of hydrogen after the reaction finishes Sodium oxide, stirred and reacted for 6 hours, then added 200 ml of water, extracted three times with dichloromethane, each 50 ml, combined the organic phases, backwashed the organic layer with 5% brine, each 50 ml, and dried with potassium carbonate, Filter, evaporate the solvent to dryness, and obtain 9 grams of reaction products by distillation under reduced pressure, the GC content is 98%, and the reaction equation is shown as follows:
[0044]
[0045]
Example Embodiment
[0046] Example 2:
[0047] Preparation of compounds with structural formula (9)
[0048]
[0049] Get 10 grams of compounds shown in structural formula (1), add catalytic amount of p-toluenesulfonic acid, add 11 grams of triethyl orthoformate, react at room temperature for 15 hours, and add 2 grams of hydrogen after the reaction is completed. Sodium oxide, stirred and reacted for 7 hours, then added 200 ml of water, extracted three times with dichloromethane, each 50 ml, combined the organic phases, backwashed the organic layer with 5% brine, each 50 ml, and dried with potassium carbonate, Filtration, evaporation of solvent, distillation under reduced pressure to obtain the reaction product of 10 grams, the GC content is 97%, and the reaction equation is shown as follows:
[0050]
[0051]
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