1,2-bis(trimethylsilyloxy)cyclohexene, and preparation method thereof
A technique for preparing bistrimethylsiloxycyclohexene and its preparation technology, which is applied in the field of 1,2-bistrimethylsiloxycyclohexene and its preparation technology, and can solve potential safety hazards, no analytical methods, and post-processing Deal with hidden dangers in the process and other issues to achieve the effect of avoiding hidden dangers
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Example Embodiment
[0024] Embodiment one:
[0025] A kind of 1,2-bistrimethylsiloxycyclohexene and its preparation process, comprising the steps of:
[0026] 1) Under the protection of dry nitrogen, sequentially introduce dry anhydrous toluene, trace amount of benzophenone and sodium metal into the reaction kettle equipped with the reaction substrate 1,6-diethyl adipate, and stir thoroughly , the reaction solution is dark blue; wherein the addition of anhydrous toluene and traces of benzophenone is a corresponding 2L solvent per mole of the reaction substrate, and the addition of metallic sodium is 4 times the molar amount of the reaction substrate;
[0027] 2) After heating up to 50°C, add the reaction substrate 1,6-diethyl adipate and the molar amount of 1,6-diethyl adipate to the reactor sequentially or simultaneously. Times of trimethylchlorosilane;
[0028] 3) After dripping, heat and stir for 3-4 hours, wait until the dark blue color of the reaction solution disappears, then stir for 1 hour
Example Embodiment
[0031] Embodiment two:
[0032] A kind of preparation chemical equation of 1,2-bistrimethylsiloxy cyclohexene is:
[0033] .
[0034]
[0035] A kind of 1,2-bistrimethylsilyloxycyclohexene and preparation technology thereof, specifically comprises the following steps:
[0036] 1) Under the protection of dry nitrogen, add 200ml of dry solvent toluene and 0.05g of benzophenone to a 1000ml three-necked flask in sequence, and then add 9.20g (0.40mol) of sodium metal in batches; after fully stirring, at this time The solution in the reaction bottle is dark blue;
[0037] 2) Then, after raising the temperature to 50°C, add 20.23g (0.1mol) of 1,6-diethyl adipate and 43.46g (0.40mol) of trimethylchlorosilane sequentially dropwise into the three-necked flask;
[0038] 3) After dropping, react at 50°C for 3 to 4 hours, wait until the dark blue color of the reaction solution disappears completely, then stir for 1 hour; stop stirring, filter out insoluble matter (NaCl, about 23.35g
Example Embodiment
[0041] Embodiment three:
[0042] 1) Under the protection of dry nitrogen, add 800ml of dry solvent toluene and 0.1g of benzophenone to a 2000ml three-necked flask in sequence, and then add 36.80g (1.6mol) of sodium metal in batches; after fully stirring, at this time The solution in the reaction bottle is dark blue;
[0043] 2) Then, after raising the temperature to 50°C, add 80.90g (0.4mol) of diethyl 1,6-adipate and 130.37g (1.6mol) of trimethylchlorosilane dropwise into the three-necked flask at the same time;
[0044] 3) After dropping, react at 50°C for 3 to 4 hours, wait until the dark blue color of the reaction solution completely disappears, then stir for 1 hour; stop stirring, filter out the insoluble NaCl (about 93.56g after drying);
[0045] 4), the filtrate is concentrated, and the by-product trimethylethoxysilane (TMSOEt, about 94.55g, boiling point 75-76°C) and solvent toluene are sequentially distilled;
[0046] 5) Afterwards, distill under reduced pressure, c
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