化工社化工社 化学情報印刷レポート · 研究参考用
Ammonia → Ethyl 5-methyl-4-oxo-2-(thiophen-3-ylmethyl)-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Diethyl 5-amino-3-methylthiophene-2,4-dicarboxylate | HCID 78537 | — |
| 反応物 | 3-Thienylacetonitrile | HCID 83730 | — |
| 反応物 | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| 生成物 | Ethyl 5-methyl-4-oxo-2-(thiophen-3-ylmethyl)-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylate | HCID 68664667 | — |
反応手順
515 Milligrams of diethyl 5-amino-3-methylthiophene-2,4-dicarboxylate and 296 mg of 3-thiopheneacetonitrile were added to 8 mL of 4N hydrogen chloride-dioxane solution and stirred for 10 hours. Thereafter the liquid reaction mixture was poured on ice, and its pH was adjusted to 8-9 with 25% aqueous ammonia. Whereupon precipitated crystals were recovered by filtration and washed first with water, and then with hexane. The crude crystals were recrystallized from a liquid mixture of N,N-dimethylformamide and cyclohexane, to provide 397 mg of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08377944B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-c9af8f1317034c27b6e3a3a0c5a95503 |
| 出典メモ | uspto-grants-2013_02 |