참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 반응물 | Hydrazinecarboxaldehyde, 2-(4-aminophenyl)- | HCID 113189 | — |
| 반응물 | HCID 178418535 | HCID 178418535 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 178418537 | HCID 178418537 | 25.4% |
반응 단계
In 50 ml of dimethylformamide were dissolved 11.1 g of 1-(3-carboxyphenyl)-5-mercaptotetrazole and 7.6 g of 4-(2-formylhydrazino)aniline, and a solution of 10.3 g of dicyclohexylcarbodiimide in 10 ml of dimethylformamide was added dropwise to the solution at 0° C. in a nitrogeneous atmosphere over about 30 minutes. After the addition, the mixture was stirred at room temperature for 3 hours. The precipitated dicyclohexylurea was separated by filtration, and the filtrate was added to 500 ml of ice-water while stirring. The thus precipitated crystals were filtered, washed with water and dispersed in 100 ml of hot methanol. The dispersion was allowed to cool to room temperature and filtered. The filtrate was washed with methanol to obtain 4.5 g of the desired compound. Melting point: 202° C. (with decomposition).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04724199 |
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| 출처 데이터셋 | uspto-grants-1988_02 |
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| ORD ID | ord-91b5da6b753c4d87a85d7b0c1e08baeb |
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| 출처 메모 | uspto-grants-1988_02 |
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