참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 7-Amino-4-hydroxy-2-naphthalenesulfonic acid | HCID 6868 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 2,4,6-Trifluoropyrimidine | HCID 69677 | — |
| 생성물 | Sulfanilic acid | HCID 8479 | — |
| 생성물 | Sodium Nitrite | HCID 23668193 | — |
반응 단계
47.8 parts of 2-amino-5-hydroxynaphthalene-7-sulfonic acid are stirred into 500 parts of water at 25° C. and are dissolved by the addition of 22 parts of a 30% by weight solution of sodium hydroxide. To this solution is added 26.8 parts of 2,4,6-trifluoropyrimidine dropwise over a 30 minute period. At the same time a 20% of sodium carbonate solution is added to this mixture continuously in order to maintain the pH of the mixture at 4-5. The reaction temperature is increased to 40-45° C. The end point of the reaction is determined using chromatographic techniques. The resultant suspension is cooled to 20-25° C. and poured onto a diazonium salt solution which is formed of 34.6 parts of 4-aminobenzene-sulfonic acid and 50 parts by volume of 4 N sodium nitrite solution at 0-5° C. and a pH of 1. During the coupling reaction the pH is maintained at 6-7 by continuously adding 20% sodium carbonate solution. The monoazo compound thus formed is salted-out using conventional methods, filtered and dried at 60° C. under vacuum. The product has the formula ##STR8##
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06127531 |
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| 출처 데이터셋 | uspto-grants-2000_10 |
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| ORD ID | ord-eb60c21061aa4b44b73c10feacf3286d |
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| 출처 메모 | uspto-grants-2000_10 |
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