A kind of synthetic method of spiro compound 2,4,8,10-tetracarbonyl-3,9-dioxaspiro[5,5]undecane
A technology of spiro compound and dioxaspiro, applied in the field of synthesis of spiro compound 2,4,8,10-tetracarbonyl-3,9-dioxaspiro[5,5]undecane, Achieve the effect of solving poor mechanical properties, reducing residual stress, and simple and convenient synthesis method
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Embodiment 1
[0036] A spiro compound 2,4,8,10-tetracarbonyl-3,9-dioxaspiro[5,5]undecane, its molecular formula is C 9 h 8 o 6 , the structural formula is
[0037] The synthesis method of the spiro compound 2,4,8,10-tetracarbonyl-3,9-dioxaspiro[5,5]undecane, the specific steps are as follows:
[0038] (1) Preparation of 1,3-magnesium dibromide-2,2-bis(magnesium bromide methyl)propane
[0039] According to the molar ratio of 1:6, weigh 1,3-dibromo-2,2-bis(bromomethyl)propane and magnesium chips; 0.5wt% of the total mass of propane takes by weighing initiator, and initiator is the mixture of iodine and ethyl bromide, and the weight ratio of the two is 1:1; Measure solvent tetrahydrofuran according to 5 times of reactant volume, standby; All reactant All need to be dewatered, and the water content should be controlled below 500ppm;
[0040]In a dry four-necked flask with a nitrogen inlet, a condenser tube (the outlet is connected to a calcium chloride drying tube), a thermometer, and a ...
Embodiment 2
[0046] A kind of synthetic method of spiro compound 2,4,8,10-tetracarbonyl-3,9-dioxaspiro[5,5]undecane, the specific steps are as follows:
[0047] (1) Preparation of 1,3-magnesium dibromide-2,2-bis(magnesium bromide methyl)propane
[0048] Except that the molar ratio is 1:5, weigh 1,3-dibromo-2,2-bis(bromomethyl)propane and magnesium chips; ) 0.8wt% of the total mass of propane takes by weighing initiator, and initiator is the mixture of iodine and ethyl bromide; Measures solvent tetrahydrofuran according to 4 times of reactant volume, all the other carry out experiment identically with (1) among the embodiment 1;
[0049] Except that the microwave reaction time is 0.7h, the microwave reaction temperature is 45°C, and the microwave power is 800W, the experiment is the same as in Example 1 to obtain 1,3-dibromide-2,2-di(magnesium bromide base) propane.
[0050] (2) Preparation of 1,3-dicarboxy-2,2-di(acetoxy)propane
[0051] In the THF solution of above-mentioned gained 1,3...
Embodiment 3
[0055] A kind of synthetic method of spiro compound 2,4,8,10-tetracarbonyl-3,9-dioxaspiro[5,5]undecane, the specific steps are as follows:
[0056] (1) Preparation of 1,3-magnesium dibromide-2,2-bis(magnesium bromide methyl)propane
[0057] In addition to weighing 1,3-dibromo-2,2-bis(bromomethyl)propane and magnesium chips according to the molar ratio of 1:7; 1.0wt% of the total mass of propane takes by weighing the initiator, which is a mixture of iodine and ethyl bromide; except that the solvent tetrahydrofuran is measured according to 6 times of the volume of the reactant, all the others are carried out the same experiment as (1) in Example 1 ;
[0058] Except that the microwave reaction time is 0.6h, the microwave reaction temperature is 44°C, and the microwave power is 700W, the experiment is the same as in Example 1 to obtain 1,3-dibromide-2,2-bis(magnesium bromide base) propane.
[0059] (2) Preparation of 1,3-dicarboxy-2,2-di(acetoxy)propane
[0060] In the THF sol...
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