Five-membered ring phosphite compound, and preparation method and application thereof
A kind of cyclic phosphite, compound technology
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[0047] The embodiment of the present invention also provides a method for preparing a five-membered ring phosphite compound, which includes the following steps:
[0048] S10. After dissolving compound A in a non-aqueous solvent, adding phosphorus trichloride for reaction, and separating compound B;
[0049] S20. After mixing the compound B and the compound C, they are reacted at a temperature of -40°C to 60°C to separate a five-membered ring phosphite compound;
[0050] Wherein, the reactant A is selected from: and / or The reactant C is selected from: and / or
[0051] Where R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 , R 10 , R 11 , R 12 , R 13 , R 14 , R 15 , R 16 , R 17 And R 18 They are independently selected from: hydrogen, alkyl, alkenyl, alkynyl, alkoxy, alkynyloxy, alkenyloxy, silyl, siloxane, arylsilyl, arylsilyl, haloalkyl , Phenyl, biphenyl, naphthyl, pyridyl, thienyl, halogenated phenyl, halogenated biphenyl, phenol, alkyl-containing phenol, alkenyl-containing...
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[0091] Example 1
[0092] In order to be able to compare the preparation processes of the products more intuitively in parallel comparison, the same self-made compound B (namely compound B prepared in Example 1) is used in Examples 2 to 33 of the present invention. The specific preparation process includes:
[0093] ① At room temperature, add 310g ethylene glycol (reactant A) and 350g anhydrous dichloromethane (non-aqueous solvent) into a three-necked flask with a volume of 2000mL in a fume hood, then cool to 0°C, continue stirring for 0.5h, At this time, the solution is colorless and transparent, and the three-necked bottle is connected to an external gas absorption device.
[0094] ② 700g of phosphorus trichloride dissolved in 300g of anhydrous dichloromethane was slowly added to the three-necked flask via a dropping funnel, and the dropping rate was controlled to be 1 drop / sec. With the continuous dropping of the dichloromethane solution of phosphorus trichloride, the reaction em...
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[0097] Example 2
[0098] Compound 1 ( Preparation of bis(1,3,2-dioxaphospholane) glycol ester):
[0099] Add 400g of dichloromethane (solvent, which has the same function as the aforementioned non-aqueous solvent, can be used selectively) and 62g of ethylene glycol (reactant C) into a 1000mL three-necked flask at room temperature. The solution is colorless and transparent. The three-necked flask is connected An external gas absorption device was connected, and then 300g of compound B prepared in Example 1 was slowly added to a 1000 mL three-necked flask via a dropping funnel, the dropping rate was controlled to 1 drop / sec, and the reaction temperature was 0°C. With the dropping of compound B, A large amount of heat is released and a large amount of HCl gas is released. After all the drops are completed, the solution is colorless and transparent (compound B is dropped for 1.5 hours), then the reaction is slowly raised to room temperature and stirring is continued for 12 hours, and...
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