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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
In 40 ml of acetonitrile was dissolved 516 mg of thiourea. In the solution was suspended 2.5 g of 2-bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)-ethanone hydrobromide. To the suspension was added dropwise slowly 0.95 ml of triethylamine while stirring. The mixture was stirred for 3 hours at a refluxing temperature, which was then left standing for cooling. Precipitating crystals were collected by filtration. The crystals were washed with an aqueous solution of saturated hydrogen carbonate, water, ethanol and ethylether in that order, followed by drying. The crystals were recrystallised from tetrahydrofuran to yield 1.5 g (90%) of 2-amino-4-(4-methoxyphenyl)-5-(3-pyridyl)-1,3-thiazol, m.p. 265°-266° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04612321 |
| 出典データセット | uspto-grants-1986_09 |
| ORD ID | ord-474e362800e249e193c25c2149262056 |
| 出典メモ | uspto-grants-1986_09 |