関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | Triethyloxonium tetrafluoroborate | HCID 2723982 | — |
| 反応物 | 5-Methyl-5-phenyl-3-phenylamino-2-thioxothiazolidin-4-one | HCID 12056392 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 2-Hydroxyimino-5-methyl-5-phenyl-3-phenylaminothiazolidine-4-one | HCID 86588497 | 70.2% |
反応手順
5-Methyl-5-phenyl-3-phenylamino-2-thioxothiazolidin-4-one (0.3 g) was added to a 1M methylene chloride solution of triethyloxonium tetrafluoroborate (1 ml) at room temperature with stirring. After stirring the mixture for 24 hrs hydroxylamine hydrochloride (0.1 g) and triethylamine (0.3 g) in methanol (10 ml) were added at 0° C. The reaction mixture was again stirred for 2 hrs at room temperature followed by evaporation of the solvents under reduced pressure. The residue was added to ice water and then extracted with ethyl acetate. The ethyl acetate solution was dried over anhydrous ethyl acetate and the solvent was then evaporated under reduced pressure. The residue was purified by column chromatography (ethyl acetate-n-hexane, ½) to yield 2-hydroxyimino-5-methyl-5-phenyl-3-phenylaminothiazolidine-4-one (0.21 g) having a melting point of 62-63° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06713629B2 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-bc5d0e561d0248559f5605bfeb83b1ff |
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| 出典メモ | uspto-grants-2004_03 |
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