Preparation of Cyclic Siloxazanes

Murray, John; Griffith, Robert K.

doi:10.1021/jo01028a054

Cited by 20 publications

(5 citation statements)

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“…To compare two deprotection methods, the standard and the new one, in terms of the silicate content, we quantitatively analyzed by IR spectroscopy the dry residues obtained after the evaporation of either ammonia solution or the neutral eluate from the underivatized CPG. It is known that the prominent band in the IR spectra in the range 1050-1100 cm -1 corresponds to the Si-O-Si stretch vibrations (13,14). Taking into account that the amount of the CPG support was the same with both procedures, we can directly compare the band intensities from two samples to estimate quantitatively the silicate contamination.…”

Section: Resultsmentioning

confidence: 99%

Advanced method for oligonucleotide deprotection

Surzhikov

Timofeev

Chernov

et al. 2000

Nucleic Acids Research

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A new procedure for rapid deprotection of synthetic oligodeoxynucleotides has been developed. While all known deprotection methods require purification to remove the residual protective groups (e.g. benzamide) and insoluble silicates, the new procedure based on the use of an ammonia-free reagent mixture allows one to avoid the additional purification steps. The method can be applied to deprotect the oligodeoxynucleotides synthesized by using the standard protected nucleoside phosphoramidites dG(iBu), dC(Bz)and dA(Bz).

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Section: Resultsmentioning

confidence: 99%

Advanced method for oligonucleotide deprotection

Surzhikov

Timofeev

Chernov

et al. 2000

Nucleic Acids Research

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“…Di-tert-butyl fumarate and1,5-dichloro-1,1,5,5-tetramethyl-3, 3-diphenyl-trisi1oxane were prepared according to the literature procedures [13][14].…”

Section: Methodsmentioning

confidence: 99%

Preparation and Characterization of Degradable Poly(silyl ester) and the Self-Crosslinking Reaction of Poly(silyl ester) without Solvent

Zhou

Han

Tang

2010

AMR

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The new poly(silyl ester) has been prepared by the polycondensation reaction of 1,5-dichloro-1,1,5,5-tetramethyl-3,3-diphenyl-trisi1oxane with di-tert-butyl fumarate by the elimination of tert-butyl chloride as a driving force. To investigate the self-crosslinking reaction of the unsaturated poly(silyl ester), poly(1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane) was self- crosslinked in the presence of 2, 2'-azobis(isobutyronitri1e) (AIBN) as a radical initiator without solvent. After the self-crosslinking, the unsaturated poly(silyl ester), which was viscous liquids, turned into solid product. The characterization of the poly(silyl ester) and the self-crosslinked product included 1H-NMR spectroscopy, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). Comparisons were made between the linear poly(silyl ester) and the self-crosslinked products. It was found that after crosslinking, the important resonance signal for ethenylene (C=C) of the poly(silyl ester) reduced, which show that the crosslinking reaction is carried out. The self-crosslinked product exist the structures of linear isomer and four-membered ring isomer. The glass-transition temperatures of the self-crosslinked poly(silyl ester) was higher than that of the uncrosslinked poly(silyl ester), and the thermal stability of the self-crosslinked poly(silyl ester) was better than that of uncrosslinked poly(silyl ester).

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“…tert ‐Butyl alcohol was obtained from Tianjin Reagent Factory and distilled in the presence of sodium. Di‐ tert ‐butyl fumarate, 1,5‐dichloro‐1,1,5,5‐tetramethyl‐3,3‐diphenyltrisiloxane, and 1,3‐dichlorotetramethyldisiloxane were prepared according to literature procedures 14–16…”

Section: Methodsmentioning

confidence: 99%

Crosslinking of poly(silyl ester)s containing fumaryloxyl units in the main chain and characteristics of the crosslinked products

Han

Liu

Zhou

et al. 2007

J of Applied Polymer Sci

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Two unsaturated poly(silyl ester)s that contained innoxious fumaryloxyl units in the main chain were prepared by the polycondensation reaction of 1,5-dichloro-1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane or 1,3-dichlorotetramethyldisiloxane with di-tert-butyl fumarate under nitrogen at 1008C for 1-3 days. To investigate the crosslinking reaction of the unsaturated poly(silyl ester)s, the two unsaturated poly(silyl ester)s were crosslinked in the presence of 2,2 0 -azobisisobutyronitrile as a radical initiator. After the crosslinking, the unsaturated poly(silyl ester)s, which were viscous liquids, turned into solid products. The characterization of the two poly(silyl ester)s and the crosslinked products included infrared spectroscopy, 1 H-NMR spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. Comparisons were made between the linear poly(silyl ester)s and the crosslinked poly(silyl ester)s. After the crosslinking, the important resonance signal for ethenylene (C¼ ¼C) disappeared, and this showed that the crosslinking reaction was carried out progressively. The glass-transition temperatures of the crosslinked poly(silyl ester)s were higher than those of the uncrosslinked poly(silyl ester)s, and the thermal stability of the crosslinked poly(silyl ester)s was better than that of uncrosslinked poly(silyl ester)s.

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Preparation of Cyclic Siloxazanes

Cited by 20 publications

References 0 publications

Advanced method for oligonucleotide deprotection

Advanced method for oligonucleotide deprotection

Preparation and Characterization of Degradable Poly(silyl ester) and the Self-Crosslinking Reaction of Poly(silyl ester) without Solvent

Crosslinking of poly(silyl ester)s containing fumaryloxyl units in the main chain and characteristics of the crosslinked products

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