참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 반응물 | Triethyloxonium tetrafluoroborate | HCID 2723982 | — |
| 반응물 | 5-Methyl-5-phenyl-3-phenylamino-2-thioxothiazolidin-4-one | HCID 12056392 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 2-Hydroxyimino-5-methyl-5-phenyl-3-phenylaminothiazolidine-4-one | HCID 86588497 | 70.2% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06713629B2 |
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| 출처 데이터셋 | uspto-grants-2004_03 |
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| ORD ID | ord-bc5d0e561d0248559f5605bfeb83b1ff |
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| 출처 메모 | uspto-grants-2004_03 |
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