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Sodium Hydroxide → 1H-Purine-2,6-dione, 3,7-dihydro-8-(2-(3-bromophenyl)ethenyl)-1,3-diethyl-, (E)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3-(3-Bromophenyl)acrylic acid | HCID 36251 | — |
| 反応物 | 5,6-Diamino-1,3-diethyluracil | HCID 4572133 | — |
| 反応物 | 1-(3-Diethylaminopropyl)-3-ethylcarbodiimide hydrochloride | HCID 9964512 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1H-Purine-2,6-dione, 3,7-dihydro-8-(2-(3-bromophenyl)ethenyl)-1,3-diethyl-, (E)- | HCID 6448930 | 51.1% |
反応手順
3-Bromocinnamic acid (2.52 g, 11.1 mmol) and 3-(3-diethylaminopropyl)-1-ethylcarbodiimide hydrochloride (2.90 g, 15.2 mmol) were added to a solution of 5,6-diamino-1,3-diethyluracil (2.0 g, 10.1 mmol) in a dioxane (34 ml)-water (68 ml) mixture, and the resulting mixture was stirred at room temperature for 40 minutes while keeping the pH at 5.5. A 4N aqueous solution of sodium hydroxide was added thereto to adjust the pH to >14, and the mixture was heated under reflux for 20 minutes. After cooling, the mixture was neutralized and the precipitated crystals were collected by filtration. The obtained crude crystals were recrystallized from tetrahydrofuran/water to give 2.01 g (yield 37%) of Compound g as pale green plates.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05670498 |
| 出典データセット | uspto-grants-1997_09 |
| ORD ID | ord-e21f30852c764a038034e8861ee1b35c |
| 出典メモ | uspto-grants-1997_09 |