참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | methyl (2E)-2-hydroxyimino-2-(2-phenoxyphenyl)acetate | HCID 88276687 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | (E)-2-(Hydroxyimino)-N-methyl-2-(2-phenoxyphenyl)acetamide | HCID 9816878 | 61% |
반응 단계
To crude E-a-hydroxyimino-2-phenoxyphenylacetic acid methyl ester (39.6 g, 0.0747 mole, purity: 51.2%) were added methanol (100 ml) and 40% aqueous solution of methylamine (15.45 g, 0.199 mole) and the mixture was stirred at room temperature for 15 hours. Then, 40% aqueous solution of methylamine (7.73 g, 0.0995 mole) was added to the mixture which was stirred in an oil bath at 70° C. for 6 hours. After completion of the reaction, water (200 ml) and toluene (100 ml) were added to the reaction mixture, which was stirred with ice cooling for one hour. The precipitated crystals were filtered off and recrystallized (methanol/toluene) to obtain E-2-hydroxyimino-N-methyl-2-(2-phenoxyphenyl)acetamide (12.31 g, yield: 60.1%) as colorless crystals (melting point: 183°-184.5° C.).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05488159 |
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| 출처 데이터셋 | uspto-grants-1996_01 |
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| ORD ID | ord-96ca491ac0e4457f970b189090d63d42 |
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| 출처 메모 | uspto-grants-1996_01 |
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