JP5116245B2 - 自動分析装置に用いる検量線作成用化合物 - Google Patents
自動分析装置に用いる検量線作成用化合物 Download PDFInfo
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- 0 **(*c(ccc(Br)c1)c1[Tl])c(cc1)cc(Cl)c1F Chemical compound **(*c(ccc(Br)c1)c1[Tl])c(cc1)cc(Cl)c1F 0.000 description 1
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有機ハロゲンおよび硫黄の一括自動分析における検量線作成用化合物の開発、東京都立産業技術研究所、研究報告第6号(2003)
N−(2’−ヨウ化−4’−臭化フェニル)−3−塩化−4−フッ化ベンゼンスルホンアミドの合成
2−ヨウ化−4−臭化−アニリン1.00g(3.37mmol)をピリジン3mlに溶解し、これに対して3−塩化−4−フッ化−ベンゼンスルホニルクロリド1.00g(4.40mmol)をピリジン4mLに溶解した溶液を氷冷下で攪拌しながら約30分にわたって滴下した。滴下後室温で3日間静置し、反応液を1mol/L塩酸溶液中に注ぎ、沈澱物を濾過し、水で洗浄した。沈澱物をカラムクロマトグラフで分離精製後、再結晶を行って精製した。白色結晶(融点133oC)が収率43%で得られた。得られた目的生成物は下記IR,NMR並びに元素分析によって前記構造式を有するN−(2’−ヨウ化−4’−臭化フェニル)−3−塩化−4−フッ化ベンゼンスルホンアミドであることが示された。
IR: 3265cm-1
N-H, 1170cm-1 S=O
NMR: 6.75(1H, N-H), 7.20(1H, aromatic), 7.46〜 7.60(3H, aromatic), 7.82 (1H, aromatic), 7.85(1H,
aromatic)
元素分析値 理論値 C:29.38% H:1.44% N:2.86%
分析値 C:29.54% H:1.63% N:2.83%
図1にその概略を示す有機ハロゲン硫黄微量分析装置YS−10(ヤナコ機器開発研究所製)を用い前記N−(2’−ヨウ化−4’−臭化フェニル)−3−塩化−4−フッ化ベンゼンスルホンアミドによってF,CL,BR,IおよびSについての検量線を同時に作成した。図1に示す装置の燃焼管にN−(2’−ヨウ化−4’−臭化フェニル)−3−塩化−4−フッ化ベンゼンスルホンアミドを入れて950oCの高温で燃焼させてガス化し、吸収液(NaHCO3+H2O2+ヒドラジン)に吸収させ、イオンクロマトグラフ系のカラム(Shodex Si-90: 4E)に展開液と共に導入して分析したところ、図2に示すようにF、Cl、Br、IおよびSのピークが夫々の位置に存在するイオンクロマトグラムが得られた。
前記のようにして得られたN−(2’−ヨウ化−4’−臭化フェニル)−3−塩化−4−フッ化ベンゼンスルホンアミドによる検量線を用いて各種の実際の試料を分析したところ、表1に示す値(%)が得られ、これら分析値は市販の検量線作成化合物を用いて同一条件で試料を分析した場合の値の差が許容範囲内にあり、こゝで用いた試料は分析の結果ヨウ素を含んでいなかった。
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JP5572459B2 (ja) * | 2010-07-05 | 2014-08-13 | 地方独立行政法人東京都立産業技術研究センター | 4種のハロゲン及び硫黄分析用の標準物質及びその製造方法 |
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ATE311363T1 (de) * | 1999-01-13 | 2005-12-15 | Warner Lambert Co | Sulfohydroxamsäure and sulfohydroxamate und ihre verwendung als mek-inhibitoren |
WO2001005393A2 (en) * | 1999-07-16 | 2001-01-25 | Warner-Lambert Company | Method for treating chronic pain using mek inhibitors |
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