참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 3-Nitrosalicylic acid | HCID 6807 | — |
| 반응물 | 5-Chlorosalicylic Acid | HCID 9447 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 5-Chloro-2-hydroxy-3-nitrobenzoic acid | HCID 412078 | — |
반응 단계
The following procedure demonstrates the preparation of compound 1 with X=5−Cl, with comparable procedures being useful for obtaining related compounds having different X. A solution suspension of 10 g of 5-chlorosalicylic acid in 50 ml glacial acetic acid was cooled in an ice bath until the solvent began to freeze. The bath was exchanged to a room temperature water bath and 4.47 g of 90% fuming nitric acid (1:1 equivalent) in 3 ml glacial acetic acid was added dropwise. After addition was complete, the mixture was stirred for 150 minutes at room temperature (R. T.) in the water bath. It was then poured into 120 ml of ice. and water and stirred in an ice bath for 30 minutes. The precipitated solid was collected by filtration and air-dried overnight.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06297401B1 |
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| 출처 데이터셋 | uspto-grants-2001_10 |
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| ORD ID | ord-62eb4662f9b34b4b92a6d0c52a31b0c7 |
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| 출처 메모 | uspto-grants-2001_10 |
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