ChemicalBook CAS DataBase List 3-Methacryloxypropylmethyldimethoxysilane

3-Methacryloxypropylmethyldimethoxysilane synthesis

4synthesis methods

Product Name:3-Methacryloxypropylmethyldimethoxysilane
CAS Number:14513-34-9
Molecular formula:C10H20O4Si
Molecular Weight:232.35

5536-61-8 Synthesis

5536-61-8
283 suppliers
$6.00/10g

18171-19-2
265 suppliers
$7.00/5g

3-Methacryloxypropylmethyldimethoxysilane

14513-34-9
209 suppliers
$9.00/25g

Yield: 94.7%

Reaction Conditions:

with 2,6-di-tert-butyl-4-methyl-phenol;tetrabutyl phosphonium bromide in N,N-dimethyl-formamide at 50 - 115; for 0.916667 h;Large scale;Reagent/catalyst;Temperature;

Steps:

1; 1; 2; 2; 3; 4
Dissolve 0.07 kg of 2,6-di-tert-butyl-p-cresol in DMF (N, N-dimethylformamide), preheat the synthesis kettle with stirring to 50 ° C, and put 150 kg of γ-chloropropylmethyldi With methoxysilane and 100 kg of DMF, turn on the stirring, heat up to 95 ° C, and add 0.88kg of tetrabutylphosphonium bromide catalyst and 89kg of sodium methacrylate, stir well. When the reaction temperature stabilizes at 115 ° C, control the reaction time to 55min. After the heat preservation was completed, the temperature was lowered to 60 ° C or lower to obtain a preliminary γ-methacryloxypropylmethyldimethoxysilane.The γ-methacryloxypropylmethyldimethoxysilane initial product obtained by the reaction was introduced into a centrifuge and filtered to obtain 275 kg of a crude γ-methacryloxypropylmethyldimethoxysilane and Sodium chloride by-product.Put the sodium chloride by-product obtained above into the drum of a rotary vacuum dryer, after the vacuum in the drum reaches -0.095 MPa, and control the vacuum degree within -0.098Mpa, heat up to 55 ° C under vacuum, Continue heating to 95-100 ° C, dry for 4 hours under reduced pressure, cool out the salt, weigh, and package to obtain potassium chloride product.The above γ-methacryloxypropylmethyldimethoxysilane crude product was introduced into the crude steamer, after the vacuum of the crude steamer reached -0.095 MPa, and the vacuum degree was controlled within -0.098Mpa, and the temperature was slowly raised. DMF collection started when the kettle temperature rose to 55 ° C, and DMF collection ended when the kettle temperature reached 100-105 ° C.Finally, the material in the crude steamer was introduced into the retort, and the vacuum degree was controlled at -0.098 MPa. When the top temperature reached 100-130 ° C, the former fraction was collected, and when the top temperature reached 115 ° C, the finished product was collected. The top temperature rose to 140 ° C. The collected fractions were collected at the time. When no liquid was distilled off, the temperature was lowered to obtain 180 kg of a finished product of γ-methacryloxypropylmethyldimethoxysilane. The product yield was 94.7%.

References:

Anhui Guibao Silicone New Materials Co., Ltd.;Sun Jiali;Qiu Xiaokui;Chen Feng;Li Yunlong CN110467632, 2019, A Location in patent:Paragraph 0056-0074; 0084-0120

96-05-9 Synthesis