참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Benzoic acid, 2-amino-5-iodo- | HCID 72911 | — |
| 반응물 | Potassium cyanate | HCID 11378442 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 6-iodo-1H-quinazoline-2,4-dione | HCID 11380668 | 91.6% |
반응 단계
To a mixture of 25.36 g of 2-amino-5-iodobenzoic acid in 250 ml of water and 90 mL of THF was added 7.40 g of glacial acetic acid and stirred at room temperature. Then was added 7.82 g of potassium cyanate in water dropwise. Left to overnight. Added another 5.47 g of potassium cyanate. Stirred overnight. A total of 160 g of NaOH pellets were added portionwise, keeping the mixture cool in ice-water bath. The mixture was stirred at room temperature overnight. The mixture was cooled in a refrigerator and the precipitate filtered through a sintered glass funnel. The precipitate was then dissolved in water and acidified with 4N HCl. The precipitate was collected by filtration. The solid was dried in a vacuum oven to yield 25.44 g of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05436233 |
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| 출처 데이터셋 | uspto-grants-1995_07 |
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| ORD ID | ord-318027e0e75040bdb499c40da42c5e2a |
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| 출처 메모 | uspto-grants-1995_07 |
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