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-(2-phenylethyl)-1,3-thiazole-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 Bicarbonate | HCID 516892 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | (2-Phenylethyl)thiourea | HCID 735845 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-isopropyl-N-(2-phenylethyl)-1,3-thiazole-2-amine | HCID 23143255 | 51.2% |
反応手順
To a solution of 3-methyl-2-butanone (0.86 g) in methanol (10 mL) was added bromine (1.60 g) at −30° C. The mixture was allowed to warm to room temperature and stirred until the red color of bromine disappeared. To the obtained colorless solution were added sodium acetate (1.60 g) and N-(2-phenylethyl)thiourea (1.80 g) and the mixture was stirred with heating under reflux for 4 hr. A saturated aqueous sodium hydrogencarbonate solution (10 mL) was added to the reaction mixture and the mixture was concentrated. The residue was purified by silica gel chromatography (ethyl acetate:hexane=1:9-2:1 in volume ratio) to give the title compound (1.26 g, yield 51%) as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07585880B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-7620a1798ae04af1b931a2782f547095 |
| 出典メモ | uspto-grants-2009_09 |