Pyrimidyl polyether as well as preparation method and application thereof
A technology of pyrimidine-based polyether and polyether polyol, which is applied in the field of an important raw material of polyurethane foam, can solve the problems that have not occurred, and achieve the effects of reducing dosage, good fluidity, and avoiding delamination.
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Embodiment 1
[0081] (1) Add 300g of ethanol to a 1000ml three-neck flask, then add 10.21g of sodium ethoxide in batches, and stir vigorously until the sodium ethoxide is completely dissolved. Then, 218.1 g (1.1 mol) of 1-(2-guanidineethyl) azacyclooctane and 130 g (1 mol) of ethyl acetoacetate were respectively added into the flask, and refluxed at 82° C. for 10 h. Add 30% hydrochloric acid, neutralize to Ph4-5, filter to obtain the crude compound C1, and recrystallize with ethanol to obtain 207g of pyrimidine derivative C1 with a purity of 99.5% and a yield of 78%.
[0082]
[0083] (2) The secondary amine group in the pyrimidine derivative directly initiates the ring-opening polymerization of propylene oxide: add 132g (0.5mol) of compound C1 into a 3L white steel reactor, and use N 2 After the replacement is qualified, the temperature of the reaction kettle is raised to 100°C, and propylene oxide (290g, 5mol) is continuously added dropwise to the kettle, and at the same time, the mixe...
Embodiment 2
[0086] (1) Add 400g of isopropanol to a 1000ml three-necked flask, then add 20.52g of sodium isopropoxide in batches, and stir vigorously after the sodium isopropoxide is completely dissolved. Then, 396 g (1.5 mol) of dodecylguanidine hydrochloride and 144 g (1 mol) of ethyl propionoacetate were respectively added into the flask, and the mixture was refluxed at 82° C. for 10 h. Add 30% hydrochloric acid, neutralize to Ph4-5, filter to obtain the crude compound J, and recrystallize with isopropanol to obtain 265.2g of pyrimidine derivative C2 with a purity of 99.5% and a yield of 85%.
[0087] The structural formula of gained pyrimidine derivative is:
[0088]
[0089] (2) The secondary amine group in the pyrimidine derivative directly initiates tetrahydrofuran for ring-opening polymerization: add 187.2 g (0.6 mol) of compound C2 into a 2L white steel reactor, and use N 2 After the replacement is qualified, the temperature of the reaction kettle is raised to 130°C, and tetr...
Embodiment 3
[0093] (1) Add 600g of K to a 1000ml three-necked flask 2 CO 3 solution (10% concentration), and then respectively add 113.27g (1.3mol) 1-ethylguanidine and 192.21g (1mol) ethyl benzoylacetate into the flask, and reflux at 100°C for 4h. Add 30% hydrochloric acid, neutralize to Ph4-5, filter to obtain the crude compound C3, and recrystallize with n-butanol to obtain 176.3g of pyrimidine derivative C3 with a purity of 98.7% and a yield of 82%.
[0094] The structural formula of gained pyrimidine derivative is:
[0095]
[0096] (2) The secondary amine group in the pyrimidine derivative directly initiates the ring-opening polymerization of propylene oxide: add 129g (0.6mol) of compound C3 into a 5L white steel reactor, and use N 2 After the replacement is qualified, the temperature of the reaction kettle is raised to 115°C, and propylene oxide (1044g, 18mol) is continuously added dropwise into the kettle. The pressure is reduced to -0.05Mpa, and the heat preservation is con...
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