JP2007262020A - ジシラン化合物 - Google Patents
ジシラン化合物 Download PDFInfo
- Publication number
- JP2007262020A JP2007262020A JP2006091449A JP2006091449A JP2007262020A JP 2007262020 A JP2007262020 A JP 2007262020A JP 2006091449 A JP2006091449 A JP 2006091449A JP 2006091449 A JP2006091449 A JP 2006091449A JP 2007262020 A JP2007262020 A JP 2007262020A
- Authority
- JP
- Japan
- Prior art keywords
- disilane
- disilane compound
- compound
- bond
- salt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- -1 Disilane compound Chemical class 0.000 title claims abstract description 21
- HJJDFXZAXVAOPK-UHFFFAOYSA-N [Mg]CCC=C Chemical class [Mg]CCC=C HJJDFXZAXVAOPK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 150000003839 salts Chemical class 0.000 claims description 4
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 abstract description 27
- 229910018557 Si O Inorganic materials 0.000 abstract description 9
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 abstract description 9
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 30
- 229940126062 Compound A Drugs 0.000 description 15
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000004458 analytical method Methods 0.000 description 11
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000001644 13C nuclear magnetic resonance spectroscopy Methods 0.000 description 5
- 238000005160 1H NMR spectroscopy Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 4
- 238000005481 NMR spectroscopy Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910008045 Si-Si Inorganic materials 0.000 description 3
- 229910006411 Si—Si Inorganic materials 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- JAUWOQLHLFMTON-UHFFFAOYSA-M magnesium;but-1-ene;bromide Chemical compound [Mg+2].[Br-].[CH2-]CC=C JAUWOQLHLFMTON-UHFFFAOYSA-M 0.000 description 3
- DQEUYIQDSMINEY-UHFFFAOYSA-M magnesium;prop-1-ene;bromide Chemical compound [Mg+2].[Br-].[CH2-]C=C DQEUYIQDSMINEY-UHFFFAOYSA-M 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical class [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004440 column chromatography Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 2
- 238000012844 infrared spectroscopy analysis Methods 0.000 description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 2
- 235000019341 magnesium sulphate Nutrition 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000004809 thin layer chromatography Methods 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 0 NCC1C*CC1 Chemical compound NCC1C*CC1 0.000 description 1
- YKBHBENPDUXKBK-UHFFFAOYSA-N [dimethyl(prop-2-enyl)silyl]-dimethyl-prop-2-enylsilane Chemical compound C=CC[Si](C)(C)[Si](C)(C)CC=C YKBHBENPDUXKBK-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- QUCQSWROBYLIEG-UHFFFAOYSA-M magnesium;but-1-ene;chloride Chemical compound [Mg+2].[Cl-].[CH2-]CC=C QUCQSWROBYLIEG-UHFFFAOYSA-M 0.000 description 1
- CYSFUFRXDOAOMP-UHFFFAOYSA-M magnesium;prop-1-ene;chloride Chemical compound [Mg+2].[Cl-].[CH2-]C=C CYSFUFRXDOAOMP-UHFFFAOYSA-M 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Images
Abstract
Description
シリコンで発光ダイオードや半導体レーザーができればこれらの問題点が解決されるだけでなく光電子集積による次世代ICの実現も可能であり、ポーラスシリコン(Si−Si結合)を発光素子に応用する研究が盛んに行われている(例えば特許文献1参照)が、その効果は充分なものではない。O−Si−Si−O結合はSi−Si結合と比較して低密度で柔軟性に富むため、フォトルミネッセンス効率を向上させることが可能である。
窒素環境下にて0℃でアリルマグネシウムブロミド200mmol(29.06g)をジエチルエーテル200mlに添加し混合した。その後、ヘキサクロロシラン18.65mmol(5.01g)を25mlジエチルエーテルに混合した溶液をアリルマグネシウムブロミド溶液に滴下し、さらに15mlのジエチルエーテルを添加した(窒素環境下)。得られた混合液を0℃にて3時間攪拌後、25℃にて18時間攪拌した。得られた混合液に5%塩酸を160ml添加し1時間攪拌後、30倍量のジエチルエーテルで抽出した。得られた抽出物は飽和炭酸水素ナトリウムで2回中和し、塩化ナトリウム飽和水溶液で2回洗浄した。得られた抽出物に脱水のため硫酸マグネシウム10gを添加し2時間放置後ろ別した。その後、ジエチルエーテルを真空下にて除去し、カラムクロマトグラフィー(Silica Gel 60<Merck製>、ヘキサン:酢酸エチル=40:1)にて精製し、ジシラン化合物Aを4.8g得た。
窒素環境下にて0℃で3−ブテニルマグネシウムブロミド200mmol(31.86g)をジエチルエーテル200mlに添加・混合した。その後、ヘキサクロロシラン18.65mmol(5.01g)を25mlジエチルエーテルに混合した溶液を3−ブテニルマグネシウムブロミド溶液に滴下し、さらに15mlのジエチルエーテルを添加した(窒素環境下)。得られた混合液を0℃にて3時間攪拌後、25℃にて18時間攪拌した。得られた混合液に5%塩酸を160ml添加し1時間攪拌後、30倍量のジエチルエーテルで抽出した。得られた抽出物は飽和炭酸水素ナトリウムで2回中和し、飽和塩化ナトリウムで2回洗浄した。得られた抽出物に脱水のため硫酸マグネシウムを添加し2時間放置後ろ別した。その後、ジエチルエーテルを真空下にて除去し、カラムクロマトグラフィー(Silica Gel 60<Merck製>、ヘキサン:酢酸エチル=40:1)にて精製し、ジシラン化合物Bを4.8g得た。
なお、1H−NMR分析、13C−NMR分析は核磁気共鳴分析装置(GMX400<JEOL製>により測定した。
ジシラン化合物A10mmol(3.02g)と水60mmol(イオン交換水1.08g)を混合後、1N塩酸200μlを添加し25℃で8時間反応させた。得られた固形分をろ別後、50mlのイオン交換水で水洗、ろ過を3回繰り返した。得られた固形分を40℃で24時間乾燥させジシランネットワーク構造物が0.99g調製された。
Claims (3)
Priority Applications (1)
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JP2006091449A JP4660410B2 (ja) | 2006-03-29 | 2006-03-29 | ジシラン化合物 |
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JP2006091449A JP4660410B2 (ja) | 2006-03-29 | 2006-03-29 | ジシラン化合物 |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2007262020A true JP2007262020A (ja) | 2007-10-11 |
JP4660410B2 JP4660410B2 (ja) | 2011-03-30 |
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JP2006091449A Active JP4660410B2 (ja) | 2006-03-29 | 2006-03-29 | ジシラン化合物 |
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH04283588A (ja) * | 1991-03-12 | 1992-10-08 | Mitsui Toatsu Chem Inc | 有機ケイ素化合物の製造法 |
JPH0853471A (ja) * | 1994-02-15 | 1996-02-27 | Shin Etsu Chem Co Ltd | クロロシラン類の炭化水素化方法 |
-
2006
- 2006-03-29 JP JP2006091449A patent/JP4660410B2/ja active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH04283588A (ja) * | 1991-03-12 | 1992-10-08 | Mitsui Toatsu Chem Inc | 有機ケイ素化合物の製造法 |
JPH0853471A (ja) * | 1994-02-15 | 1996-02-27 | Shin Etsu Chem Co Ltd | クロロシラン類の炭化水素化方法 |
Non-Patent Citations (2)
Title |
---|
JPN6010060076, Journal of the Chemical Society, Dalton Transactions.: Inorganic Chemistry, No.23, p.2537−2542 (1974). * |
JPN6010060078, Annales de Chimie, Vol.8, No.1−2, p.163−174 (1983). * |
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