化工社化工社 化学情報印刷レポート · 研究参考用
3-Methyl-2-butanone → 4-isopropyl-N-(3-methylbutyl)-1,3-thiazol-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Methyl-2-butanone | HCID 11251 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | (3-Methyl-butyl)-thiourea | HCID 2459097 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-isopropyl-N-(3-methylbutyl)-1,3-thiazol-2-amine | HCID 23083099 | 21.2% |
反応手順
A solution of 3-methyl-2-butanone (2.64 g) in methanol (30 ml) was cooled to −30° C. bromine (4.8 g) was added, and heated to room temperature with stirring. To the obtained colorless solution were added N-(3-methylbutyl)thiourea (2.92 g) and sodium acetate (2.40 g) and the mixture was stirred with heating under reflux for 2 hrs. The reaction mixture was concentrated, diluted with ethyl acetate and washed with water. The ethyl acetate layer was concentrated, and the residue was purified by silica gel column chromatography with ethyl acetate-hexane (gradient of 1:9 to 2:1 by volume ratio) to give the title compound (0.90 g, yield 21%) as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07960369B2 |
| 出典データセット | uspto-grants-2011_06 |
| ORD ID | ord-3e3b63acf6a647f381eb1d9d24bf8573 |
| 出典メモ | uspto-grants-2011_06 |