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1,2-bis(trimethylsilyloxy)cyclobutene, and preparation method thereof

A technique for preparing bistrimethylsiloxycyclobutene and its preparation technology, which is applied in the field of 1,2-bistrimethylsiloxycyclobutene and its preparation technology, and can solve potential safety hazards and post-processing safety hazards , there is no analysis method and other problems, to achieve the effect of avoiding potential safety hazards

Active Publication Date: 2015-05-06
XINYAQIANG SILICON CHEM JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the past, most of the organic reactions that directly used metallic sodium as a reagent had the following potential safety hazards: in production, there was no simple and feasible analysis method to judge whether the input metallic sodium had fully participated in the reaction
Therefore, in the post-processing process, the residual metal sodium that has not been completely reacted is often encountered, which brings great potential safety hazards to the post-processing process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of 1,2-bistrimethylsiloxycyclobutene and its preparation process, comprising the steps of:

[0025] 1) Under the protection of dry nitrogen, sequentially introduce dry anhydrous toluene, trace amount of benzophenone and metal sodium into the reaction kettle equipped with the reaction substrate 1,4-diethyl succinate, and stir thoroughly , the reaction solution is dark blue; wherein the addition of anhydrous toluene and trace amounts of benzophenone is 2L of solvent per mole of the reaction substrate, and the addition of metallic sodium is 4 times the molar amount of the reaction substrate;

[0026] 2) After heating up to 50°C, add the reaction substrate 1,4-diethyl succinate and the molar amount of 1,4-diethyl succinate 4 to the reactor sequentially or simultaneously. Times of trimethylchlorosilane;

[0027] 3) After dropping, keep warm and stir for 3-4 hours, wait until the dark blue color of the reaction solution disappears, then stir for 1 hour, filter out the...

Embodiment 2

[0031] A kind of preparation chemical equation of 1,2-bistrimethylsiloxycyclobutene is:

[0032] .

[0033] A kind of 1,2-bistrimethylsiloxycyclobutene and preparation technology thereof, specifically comprises the following steps:

[0034] 1) Under the protection of dry nitrogen, add 150ml of dry solvent toluene and 0.05g of benzophenone to a 500ml three-necked flask in sequence, and then add 4.60g (0.20mol) of sodium metal in batches; after fully stirring, at this time The solution in the reaction bottle is dark blue;

[0035] 2) Then, after raising the temperature to 50°C, add 8.71g (0.05mol) of diethyl 1,4-succinate and 21.73g (0.20mol) of trimethylchlorosilane sequentially dropwise into the three-necked flask;

[0036] 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 11.70g after drying) ;

[0037] 4), the...

Embodiment 3

[0040] 1) Under the protection of dry nitrogen, add 400ml of dry solvent toluene and 0.1g of benzophenone to a 2000ml three-necked flask in sequence, and then add 18.40g (0.8mol) of sodium metal in batches; after fully stirring, at this time The solution in the reaction bottle is dark blue;

[0041] 2) Then, after raising the temperature to 50°C, add 34.84g (0.2mol) diethyl 1,4-succinate and 86.91g (0.8mol) trimethylchlorosilane dropwise into the three-necked flask at the same time;

[0042] 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 the insoluble NaCl (about 46.80g after drying);

[0043] 4), the filtrate is concentrated, and the by-product trimethylethoxysilane (TMSOEt, about 47.20g, boiling point 75-76°C) and solvent toluene are distilled out in sequence;

[0044] 5) Afterwards, distill under reduced pressure, collect the fraction at 75-7...

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Abstract

The invention belongs to the field of chemical material production, and especially relates to 1,2-bis(trimethylsilyloxy)cyclobutene, and a preparation method thereof. Preparation chemical equation of 1,2-bis(trimethylsilyloxy)cyclobutene is represented by a formula in the invention. According to the preparation method, existing of unreacted metallic sodium residue in a reaction mixture is indicated based on a phenomenon that a blue compound is obtained via reaction of benzophenone with metallic sodium in an anhydrous solution; and a convenient and feasible method used for determining metallic sodium residual after reaction is provided, and potential safety hazards in post treatment processes are avoided completely.

Description

technical field [0001] The invention relates to the field of production and preparation of chemical materials, in particular to 1,2-bistrimethylsilyloxycyclobutene and a preparation process thereof. Background technique [0002] Organosilicon reagents were initially used in organic synthesis as a protective reagent for compounds containing hydroxyl groups. In recent years, with the rapid development of organosilicon chemical application technology research, the research on organosilicon compounds as drug synthesis reagents and drug synthesis intermediates has achieved fruitful results. Many organosilicon compounds, such as enol silyl ether, alkenyl silane, trimethyl iodosilane, phenyl silane, etc., are all organic synthesis reagents with various reactivity properties, and they have become indispensable in modern drug synthesis. important reagents and intermediates. [0003] Dienol silyl ethers are a class of very useful important reagents and important intermediates. Appl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 初亚军刘汉兴李志刚杨恵权
Owner XINYAQIANG SILICON CHEM JIANGSU
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