関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Propionic Acid | HCID 1032 | — |
| 反応物 | Sulfamic Acid | HCID 5987 | — |
| 反応物 | 2-Chloro-4-nitroaniline | HCID 8492 | — |
| 反応物 | Nitrosylsulfuric acid | HCID 82157 | — |
| 反応物 | 3-(Ethyl-phenyl-amino)-propionic acid vinyl ester | HCID 67266914 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-{[4-(2-Chloro-4-nitrophenylazo)-phenyl]-ethyl-amino}-propionic acid vinyl ester | HCID 59141510 | — |
反応手順
5.2 parts of 2-chloro-4-nitroaniline, 20 parts of propionic acid and 30 parts of acetic acid were charged and cooled to 5° C. 11.4 parts of 40% (w/w) nitrosyl sulfuric acid were added, whilst the temperature was held below 10° C. The diazotization mixture was stirred for a further 2 hrs at 5-10° C. To a separate vessel were charged 6.5 parts of 3-(ethyl-phenyl-amino)-propionic acid vinyl ester, 100 parts of methanol, 1 part sulfamic acid and 100 parts of ice. With stirring, the diazotization mixture was slowly added followed by a further 300 parts of ice. The reaction mixture was stirred over night and the product was isolated by filtration, washed with water and dried to yield 9.9 parts of 3-{[4-(2-chloro-4-nitrophenylazo)-phenyl]-ethyl-amino}-propionic acid vinyl ester. λmax=510 nm (DMF).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07871446B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-8cd0f8752a0d4b329b490afb81d525b9 |
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| 出典メモ | uspto-grants-2011_01 |
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