- A at the same time improve the N, O — double (three a silicon-based) acetamide purity and yield of production method
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The invention provides a production method for improving the purity and yield of N,O-bis(trimethyl silyl) acetamide simultaneously. The production method comprises the steps of trimethylchlorosilane preparation, charging, synthetic reaction and distillation. In the step of distillation, front cut fraction is obtained through distillation, and a finished product is obtained through distillation; in the step of trimethylchlorosilane preparation, according to the mole ratio of the trimethylchlorosilane to acetamide being 2.11-2.22:1, the trimethylchlorosilane is sucked into a trimethylchlorosilane overhead tank, and the vacuum degree of the trimethylchlorosilane overhead tank is kept 0.001-0.005 MPa before charging. According to the prepared product BSA, the product purity reaches 99.58-99.66%, the impurity number and content are reduced, and the amine content is 0.20-0.25%; the BSA once through yield reaches 93.42-93.7%, and the raw material conversion rate is high and is improved by more than 3% compared with the prior art.
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Paragraph 0046-0057; 0073-0085; 0099-0111; 0125-0137
(2018/05/24)
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- Semi-continuous process for preparing bis-silyl carboxamides
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For preparing bis-silyl carboxamides in a semi-continuous, reacting an amide or the N-trimethylsilyl derivative thereof with a silylating agent and, at the same time, extracting the bis-silyl carboxamide formed by distillation under reduced pressure.
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- Carbacephalosporin compound, their preparation and use
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Carbacephalosporin compounds of formula (I), STR1 salts thereof, processes for their synthesis and uses thereof, wherein: R1 is hydrogen, methoxy or formamido; R2 is an acyl group; CO2 R3 is a carboxy group or a carboxylate anion, or R3 is a carboxy protecting group or a pharmaceutically acceptable salt-forming group or in vivo hydrolysable ester group; R4, R5, R6 and R7 represent hydrogen or a substituent; R4 and R7 may be replaced by a chemical bond between the two carbon atoms shown; R5 and R6 may be linked together into a cyclic system. The compounds (I) have antibacterial properties.
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- BIS (TRIMETHYLSILYL) AMIDE AS NITRILE PRECURSOR
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Bis (trimethylsilyl) amides are converted into nitriles with high yields when they are treated with a catalyst (tetrabutylammonium fluoride, Lewis acids or iron phthalocyanine).
- Rigo, Benoit,Lespagnol, Charles,Pauly, Marc
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p. 347 - 348
(2007/10/02)
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