化工社化工社 化学情報印刷レポート · 研究参考用
Stannous chloride dihydrate → (4-aminophenyl)(1-methyl-1H-imidazol-5-yl)methanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | (1-Methyl-1H-imidazol-5-yl)(4-nitrophenyl)methanone | HCID 86715600 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | (4-aminophenyl)(1-methyl-1H-imidazol-5-yl)methanone | HCID 90101950 | — |
反応手順
A mixture of (1-methyl-1H-imidazol-5-yl)(4-nitrophenyl)methanone (1.30 g, 5.62 mmol, Intermediate 15: step b and tin(II)chloride dihydrate (6.54 g, 28.1 mmol) in EtOH (35 mL) was stirred at reflux for 1 hour, cooled to room temperature and evaporated in vacuo to remove most of the EtOH. The residue was poured into a 3 M aqueous NaOH/ice solution rinsing with EtOAc. The mixture was stirred at room temperature for 15 minutes then layers were separated. The aqueous layer was again extracted with EtOAc. The combined EtOAc extracts were washed with brine, dried (Na2SO4), filtered and evaporated in vacuo to provide the title compound as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09284308B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-3cfb7b3b13dd4f09b07c33441e71498c |
| 出典メモ | uspto-grants-2016_03 |