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The Kolbe-Schmitt Reaction in Aqueous Solutions. 水溶液中的Kolbe-Schmitt反应。
Nippon Kagaku Kaishi Pub Date : 2002-01-01 DOI: 10.1246/NIKKASHI.2002.467
Naoki Morinaga, M. Uchigashima, M. Rahim, K. Onishi, Kazufumi Takahashi, Y. Kosugi
{"title":"The Kolbe-Schmitt Reaction in Aqueous Solutions.","authors":"Naoki Morinaga, M. Uchigashima, M. Rahim, K. Onishi, Kazufumi Takahashi, Y. Kosugi","doi":"10.1246/NIKKASHI.2002.467","DOIUrl":"https://doi.org/10.1246/NIKKASHI.2002.467","url":null,"abstract":"The carboxylation of m-aminophenol with potassium hydrogencarbonate in aqueous solutions has been studied kinetically. The formation of 4-hydroxyanthranilic acid (4HAA) has been found for the first time in the carboxylation of m-aminophenol which gives only p-aminosalicylic acid (pAS) in the usual Kolbe-Schmitt reaction. Since 4HAA was easily decarboxylated, the product was removed from the reaction mixture after the carboxylation for 1 h at 60 °C. This method was repeated three times and 4HAA was obtained as a major product in 30.2% yield.","PeriodicalId":19311,"journal":{"name":"Nippon Kagaku Kaishi","volume":"39 1","pages":"467-469"},"PeriodicalIF":0.0,"publicationDate":"2002-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86115899","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 3
Electrochemical Reduction of Nickel(II) Hydroxide Deposited on Carbon Powder and Application to a New Activation Method for Hydrogen Storage Alloy Negative Electrodes. 碳粉沉积氢氧化镍的电化学还原及其在储氢合金负极活化新方法中的应用
Nippon Kagaku Kaishi Pub Date : 2002-01-01 DOI: 10.1246/NIKKASHI.2002.129
S. Morishita, Y. Isogai, K. Itoh, S. Towata, K. Abe
{"title":"Electrochemical Reduction of Nickel(II) Hydroxide Deposited on Carbon Powder and Application to a New Activation Method for Hydrogen Storage Alloy Negative Electrodes.","authors":"S. Morishita, Y. Isogai, K. Itoh, S. Towata, K. Abe","doi":"10.1246/NIKKASHI.2002.129","DOIUrl":"https://doi.org/10.1246/NIKKASHI.2002.129","url":null,"abstract":"水酸化ニッケル(II)の析出したカーボン粉末[Ni(OH)2/C]をカソード分極後，X線回折，磁気測定ならびにTEM観察を行った．カーボン粉末の表面に析出した水酸化ニッケル(II)の1.4%以上が電気化学的に還元されて金属ニッケル微粒子を生成した．生成したニッケル微粒子が充放電反応の活性点として作用するため，Ni(OH)2/Cの添加によって水素吸蔵合金負極の初期活性化が促進された．","PeriodicalId":19311,"journal":{"name":"Nippon Kagaku Kaishi","volume":"29 1","pages":"129-133"},"PeriodicalIF":0.0,"publicationDate":"2002-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82208934","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Regioselective Aldol Addition Reaction of Nitroalkane Dianions. 硝基烷烃双离子的区域选择性醛醇加成反应。
Nippon Kagaku Kaishi Pub Date : 2002-01-01 DOI: 10.1246/NIKKASHI.2002.475
Seiji Tanaka, K. Kawasaki, Mariko Hirao, K. Kishikawa, S. Kohmoto, Makoto Yamamoto*
{"title":"Regioselective Aldol Addition Reaction of Nitroalkane Dianions.","authors":"Seiji Tanaka, K. Kawasaki, Mariko Hirao, K. Kishikawa, S. Kohmoto, Makoto Yamamoto*","doi":"10.1246/NIKKASHI.2002.475","DOIUrl":"https://doi.org/10.1246/NIKKASHI.2002.475","url":null,"abstract":"Previously we reported regioselective formation of dianions derived from liner nitroalkanes in the presence of n-BuLi and HMPA. The formation of nitroalkane dianions either α,α- or α,β-dianions depended on the order of addition of reagents. However, the usage of a carcinogen suspected compound like HMPA is undesirable. Therefore we re-investigated the new combination of bases and aprotic dipolar solvents other than HMPA. After exploration of a variety of their combination, it was found that the combination of LDA and DMPU resulted in the formation of α,β-dianion with the best regioselectivity; the ratio of α- to β-adduct was 1 to 14 in the reaction of nitroethane with benzaldehyde.","PeriodicalId":19311,"journal":{"name":"Nippon Kagaku Kaishi","volume":"34 1","pages":"475-479"},"PeriodicalIF":0.0,"publicationDate":"2002-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89754767","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Synthesis of Cross-Linked Starch with Acrylic Acid 丙烯酸交联淀粉的合成
Nippon Kagaku Kaishi Pub Date : 2002-01-01 DOI: 10.1246/NIKKASHI.2002.359
K. Ogawa, C. Shimasaki, T. Yoshimura, S. Ono, I. Yamazaki
{"title":"Synthesis of Cross-Linked Starch with Acrylic Acid","authors":"K. Ogawa, C. Shimasaki, T. Yoshimura, S. Ono, I. Yamazaki","doi":"10.1246/NIKKASHI.2002.359","DOIUrl":"https://doi.org/10.1246/NIKKASHI.2002.359","url":null,"abstract":"","PeriodicalId":19311,"journal":{"name":"Nippon Kagaku Kaishi","volume":"87 1","pages":"359-363"},"PeriodicalIF":0.0,"publicationDate":"2002-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77607680","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 1
Kirkwood-Buff積分および揺らぎからみた1-プロパノール水溶液の構造 从Kirkwood-Buff积分和波动看1-丙醇水溶液的结构
Nippon Kagaku Kaishi Pub Date : 2002-01-01 DOI: 10.1246/NIKKASHI.2002.301
徹夫 中川
{"title":"Kirkwood-Buff積分および揺らぎからみた1-プロパノール水溶液の構造","authors":"徹夫 中川","doi":"10.1246/NIKKASHI.2002.301","DOIUrl":"https://doi.org/10.1246/NIKKASHI.2002.301","url":null,"abstract":"1-プロパノール水溶液の構造に関する知見を得るため，Kirkwood-Buff(KB)積分G11，G22，G12 (1 : 1-プロパノール，2 : 水)，1-プロパノールの濃度揺らぎN ，密度揺らぎ /N，密度揺らぎと濃度揺らぎの相関 ，両成分の密度揺らぎ / および両者の相関 / を，全濃度範囲，283.15–353.15 Kの温度範囲で算出した．KB積分は，等温圧縮率kT，過剰モルギブズエネルギーGmEおよび過剰モル体積VmEなどの熱力学量より計算した．続いて西川の方法により，KB積分の値を，各種揺らぎの値に変換した．G11, G22, N , /Nおよび / は，x1≈0.2に極大値が出現し，温度上昇とともに増大した．一方，G12， および / は同じ濃度において極小値が出現し，温度上昇とともに減少した．しかし，x1>0.3の濃度領域では，これらの温度依存性は逆転した．以上のことより，1-プロパノール水溶液の構造に関して，次のように解釈できる．x1 0.3では，温度上昇とともに1-プロパノール-水間の会合が進行する．","PeriodicalId":19311,"journal":{"name":"Nippon Kagaku Kaishi","volume":"19 1","pages":"301-307"},"PeriodicalIF":0.0,"publicationDate":"2002-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73792433","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 3
A Convenient Method of Generation of Nitrile Oxides by Iodosylbenzene and Its Reaction. 一种用碘基苯生成氧化腈的简便方法及其反应。
Nippon Kagaku Kaishi Pub Date : 2002-01-01 DOI: 10.1246/NIKKASHI.2002.471
Seiji Tanaka, Mikinao Ito, K. Kishikawa, S. Kohmoto, Makoto Yamamoto*
{"title":"A Convenient Method of Generation of Nitrile Oxides by Iodosylbenzene and Its Reaction.","authors":"Seiji Tanaka, Mikinao Ito, K. Kishikawa, S. Kohmoto, Makoto Yamamoto*","doi":"10.1246/NIKKASHI.2002.471","DOIUrl":"https://doi.org/10.1246/NIKKASHI.2002.471","url":null,"abstract":"A mild and convenient method for generation of nitrile oxide is established by iodosylbenzene oxidation of aldehyde oximes. Aldehyde oximes were converted to furoxans in almost quantitative yields via dimerization of corresponding nitrile oxides upon oxidation. When the oxidation was carried out in the presence of alkene and alkyne dipolarophiles, isoxazolines or isoxazoles were obtained in good yields.","PeriodicalId":19311,"journal":{"name":"Nippon Kagaku Kaishi","volume":"25 7-8 1","pages":"471-473"},"PeriodicalIF":0.0,"publicationDate":"2002-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85946470","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 13
Effects of Sulfate Ion on Crystal Structure and Activity for Methane Oxidation of Iron Oxide Prepared from Goethite. 硫酸盐离子对针铁矿制备的氧化铁的晶体结构和甲烷氧化活性的影响。
Nippon Kagaku Kaishi Pub Date : 2002-01-01 DOI: 10.1246/NIKKASHI.2002.11
Masanao Orihara, Suminori Tanaka, Sigeo Kawakami, K. Nakagawa, Masahiro Kato, S. Sugiyama, T. Moriga, I. Nakabayashi
{"title":"Effects of Sulfate Ion on Crystal Structure and Activity for Methane Oxidation of Iron Oxide Prepared from Goethite.","authors":"Masanao Orihara, Suminori Tanaka, Sigeo Kawakami, K. Nakagawa, Masahiro Kato, S. Sugiyama, T. Moriga, I. Nakabayashi","doi":"10.1246/NIKKASHI.2002.11","DOIUrl":"https://doi.org/10.1246/NIKKASHI.2002.11","url":null,"abstract":"ゲータイト(α-FeO(OH))を前駆物質として合成した酸化鉄を用いてメタン酸化活性試験を行った．ゲータイトは水酸化ナトリウム水溶液と硫酸鉄水溶液を混合した懸濁液の空気酸化により調製され，その熱分解により酸化鉄を得た．酸化鉄によるメタン酸化活性は硫酸イオンの存在で抑制されることがわかった．そこで，ゲータイトを硫酸に浸漬してその表面に硫酸イオン(SO42−)を存在させ，残存した硫酸イオンがゲータイトから調製された酸化鉄の結晶構造とメタン酸化活性に及ぼす影響について詳しく検討した．その結果，硫酸イオンは250 °C付近で起こるゲータイトからヘマタイト(α-Fe2O3)への相転移温度を約30 °C高温側へシフトさせることが明らかになった．また，この硫酸イオンは鉄原子に電子を供与して鉄の酸化力を減少させ，300 °Cから500 °Cの温度範囲においてメタン酸化活性を低下させ，かつメタンの部分酸化を引き起こす．さらに硫酸イオンによって，相転移して生成したヘマタイト中に多くの格子欠陥が存在し，(113l)(l : 0，1，2)面に代表される鉄原子の並びに関係する特定の面以外，すなわち酸素が関与する原子配列を乱すことがわかった．硫酸処理されたゲータイトから得られたヘマタイトを触媒として，550 °C以上でメタン酸化活性試験を行ったところ，硫酸処理なしのゲータイトから得られたヘマタイトよりも高活性であった．550 °C以上の温度においてヘマタイト表面の硫酸イオンは脱離するが，硫酸イオンによってもたらされたヘマタイトの格子欠陥は残り，この格子欠陥が高活性の要因であると考えられる．","PeriodicalId":19311,"journal":{"name":"Nippon Kagaku Kaishi","volume":"1 1","pages":"11-18"},"PeriodicalIF":0.0,"publicationDate":"2002-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88614918","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 3
Partial Reduction of Reactive NiAl2O4 Spinel Prepared from a Sulfate Solid Solution. 硫酸盐固溶体制备活性NiAl2O4尖晶石的部分还原。
Nippon Kagaku Kaishi Pub Date : 2002-01-01 DOI: 10.1246/NIKKASHI.2002.195
K. Daimon, T. Isobe, Y. Hikichi, T. Ota
{"title":"Partial Reduction of Reactive NiAl2O4 Spinel Prepared from a Sulfate Solid Solution.","authors":"K. Daimon, T. Isobe, Y. Hikichi, T. Ota","doi":"10.1246/NIKKASHI.2002.195","DOIUrl":"https://doi.org/10.1246/NIKKASHI.2002.195","url":null,"abstract":"Al2(SO4)3–NiSO4系硫酸塩固溶体の加熱分解によって生成した高反応性のNiAl2O4スピネルの部分還元反応について調べた．マイクロ波を用いた水溶液の急速な乾固によって，NiSO4が固溶した無水Al2(SO4)3が生成した．Ni2+イオンは65 mol% (NiSO4/(NiSO4 + Al2(SO4)3))までの広い範囲にわたって無水硫酸アルミニウムの結晶格子に固溶する．この無水硫酸塩は900 °Cで分解してスピネル，酸化ニッケル，η-アルミナを生成した．Ni含有率で約20 mol%から50 mol% (NiO/(NiO + Al2O3))の範囲で，ほかの結晶相が共存することなく，スピネルの格子定数は直線的に変化した．スピネル粉末の圧密体を炭素粉末中に埋め込み，加熱して部分還元した．700 °Cまでの加熱で，NiOがスピネルから分離して，スピネル中のアルミナの高濃度化をもたらした．NiOならびにスピネルと共存する状態で，800 °C以上で金属Niが生成した．スピネルの格子定数は，スピネル中のNi含有量の減少とともに小さくなった．1200 °CまではNiO，金属Niならびにスピネルが共存したが，1300 °Cでの加熱により，α-アルミナ/金属Ni複合体が生成した．","PeriodicalId":19311,"journal":{"name":"Nippon Kagaku Kaishi","volume":"77 1","pages":"195-199"},"PeriodicalIF":0.0,"publicationDate":"2002-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81184060","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 4
Synthesis of .ALPHA.-Lithium Aluminate Fiber and Its Stability in Molten Carbonate Salt. α的合成。铝酸锂纤维及其在熔融碳酸盐中的稳定性。
Nippon Kagaku Kaishi Pub Date : 2002-01-01 DOI: 10.1246/NIKKASHI.2002.97
K. Takizawa, A. Hagiwara
{"title":"Synthesis of .ALPHA.-Lithium Aluminate Fiber and Its Stability in Molten Carbonate Salt.","authors":"K. Takizawa, A. Hagiwara","doi":"10.1246/NIKKASHI.2002.97","DOIUrl":"https://doi.org/10.1246/NIKKASHI.2002.97","url":null,"abstract":"溶融炭酸塩形燃料電池(MCFC)では，電解質保持板の補強材料としてアルミナ(Al2O3)繊維が用いられているが，経時的に腐食劣化することが知られている．電解質保持板構成材料であるアルミン酸リチウム(LiAlO2)については，長期運転でも劣化が少ないとされるα相が注目されている．そこで補強材についてもα-アルミン酸リチウムを適用することを試みた．出発物質としてγ相のアルミナ繊維を用いて炭酸リチウムとの反応を検討した結果，600–650 °Cの温度で二酸化炭素雰囲気下において繊維形状を保った良好なα-アルミン酸リチウム繊維を合成することができた．さらにこの繊維の溶融炭酸塩中における耐食性をアルミナ繊維と比較検討した．電解質保持板を模擬したα-アルミン酸リチウム粉末と繊維の混合物は，溶融炭酸塩中でもアルミナ繊維と同等の耐食性を示した．また結晶構造はα相を維持していた．これらの結果から，長期耐久性に優れた“α-アルミン酸リチウム電解質保持板”への可能性を示すことができた．","PeriodicalId":19311,"journal":{"name":"Nippon Kagaku Kaishi","volume":"1 1","pages":"97-102"},"PeriodicalIF":0.0,"publicationDate":"2002-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88749386","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Incorporation with Possible Regular Arrangement of Silver Ion in Interlayer Region of Mg/Al Layered Double Hydroxide with Interlayer Thiosulfate Ion. 银离子在Mg/Al层状双氢氧化物层间区与层间硫代硫酸盐离子的可能规则排列。
Nippon Kagaku Kaishi Pub Date : 2002-01-01 DOI: 10.1246/NIKKASHI.2002.393
E. Kanezaki, Kazuki Maeda
{"title":"Incorporation with Possible Regular Arrangement of Silver Ion in Interlayer Region of Mg/Al Layered Double Hydroxide with Interlayer Thiosulfate Ion.","authors":"E. Kanezaki, Kazuki Maeda","doi":"10.1246/NIKKASHI.2002.393","DOIUrl":"https://doi.org/10.1246/NIKKASHI.2002.393","url":null,"abstract":"あらかじめ，チオ硫酸イオンを層間に取り込んだMg/Al-LDH前駆物質を合成し，そののち前駆物質とAg+イオンとを水溶液中で反応させることにより層間にAg+イオンを取り込んだ層状複水酸化物(Ag+-LDH)を合成した．Ag+-LDHのFT-IRスペクトルの解析から，層間のAg+イオンはチオ硫酸イオンの末端硫黄原子が2個配位した直線型構造を持つことがわかった．この固体の示差熱曲線中には，前駆物質と類似した熱変化が観測されたが，幾つかのピークではAg+イオンの取り込みによりピーク温度がシフトした．また，それぞれの固体の組成式をよく支持する熱重量曲線が得られた．Ag+-LDHの粉末X線回折図には，取り込んだAg+イオン量の増加とともに，(002)回折線強度が相対的に増加した．これは，層間に取り込まれたAg+イオンが，層に平行に規則的に並んだ格子面を持つ新たな結晶格子を形成したためと考えた．","PeriodicalId":19311,"journal":{"name":"Nippon Kagaku Kaishi","volume":"75 1","pages":"393-397"},"PeriodicalIF":0.0,"publicationDate":"2002-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76559896","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 4
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