참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 1-Chloro-4-nitrobenzene | HCID 7474 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Ethyl acetohydroximate | HCID 99894 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Ethyl N-(4-nitrophenoxy)ethanimidate | HCID 71416420 | 98.5% |
반응 단계
4-Chloronitrobenzene, 136.2 g, and 111.4 g ethyl N-hydroxyacetimidate are dissolved in 216 ml DMF. The temperature is adjusted to 30° C. and 41.6 g solid NaOH is added in 8 portions keeping the temperature at 30-35° C. After one hour the temperature is adjusted to 40-45° C. and the mixture stirred for 1.5 hours. Cooling is applied and 520 ml water is fed at such a rate as to keep the temperature at ca 40° C. The slurry formed is cooled to 17° C. and filtered. The filter cake is washed with 175 ml ethanol/water 90/10 (V/V) followed by 175 ml water. Wet product, 214.5 g, corresponding to 192 g dry ethyl N-(4-nitrophenoxy)acetimidate is isolated. Yield 98.5%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08519165B2 |
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| 출처 데이터셋 | uspto-grants-2013_08 |
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| ORD ID | ord-b68e3abc518c40109589c2afa92ea91f |
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| 출처 메모 | uspto-grants-2013_08 |
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