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Triethylamine → 2-Thiazolamine, 4-(4-methoxyphenyl)-5-(3-pyridinyl)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Thiourea | HCID 2723790 | — |
| 反応物 | 2-Bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)ethanone hydrobromide | HCID 11463336 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Thiazolamine, 4-(4-methoxyphenyl)-5-(3-pyridinyl)- | HCID 3024894 | 90% |
反応手順
To a suspension of thiourea (516 mg) in acetonitrile (40 mL), was added 2-bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)ethanone hydrobromide (2.5 g), and then triethylamine (0.95 mL) was added slowly dropwise to the mixture with stirring. After addition, the mixture was stirred at reflux for 3 h. After cooling, the crude crystalline was collected by filtration. The crystalline was washed with an aqueous saturated solution of sodium hydrogen carbonate, water, ethanol, and ethyl ether, in that order, and dried. The obtained crude crystalline was recrystallized from tetrahydrofuran to give the title compound (1.5 g, yield 90%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06436966B1 |
| 出典データセット | uspto-grants-2002_08 |
| ORD ID | ord-c535df6ef80140ada17f9a41b9ee72b3 |
| 出典メモ | uspto-grants-2002_08 |