참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Ethyl chloroformate | HCID 10928 | — |
| 반응물 | 2-Fluoro-5-nitroaniline | HCID 67785 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Ethyl 2-fluoro-5-nitrocarbanilate | HCID 2754990 | 98.2% |
반응 단계
10.7 g (98.9 mmol) of ethyl chloroformate was added dropwise to a mixture of 15.0 g (94.2 mmol) of 2-fluoro-5-nitroaniline, 8.20 g (104 mmol) of pyridine and 150 ml of dichloromethane at a temperature of not higher than 5° C. Thereafter the temperature was raised to room temperature and the reaction was continued for one night. After the dichloromethane layer was separated out by adding water to the reaction mixture, the dichloromethane layer was washed with saturated saline solution and dried over anhydrous sodium sulfate. Thereafter the dichloromethane was distilled off to obtain the crude product (crystals). The crude product was washed with hexane, thereby obtaining 21.1 g of the objective product (yield: 98%) in the form of ocher crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05416236 |
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| 출처 데이터셋 | uspto-grants-1995_05 |
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| ORD ID | ord-5b7fd3a86e434faab81ec81274d3d4a9 |
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| 출처 메모 | uspto-grants-1995_05 |
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