関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Benzoic acid, 2-amino-5-iodo- | HCID 72911 | — |
| 反応物 | Potassium cyanate | HCID 11378442 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 6-iodo-1H-quinazoline-2,4-dione | HCID 11380668 | 91.6% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05436233 |
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| 出典データセット | uspto-grants-1995_07 |
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| ORD ID | ord-318027e0e75040bdb499c40da42c5e2a |
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| 出典メモ | uspto-grants-1995_07 |
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