化工社化工社 化学情報印刷レポート · 研究参考用
Ethanethiol → 7-Hydroxy-4-methyl-3-pyridin-4-yl-chromen-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanethiol | HCID 6343 | — |
| 反応物 | Aluminum bromide | HCID 24409 | — |
| 反応物 | 7-Methoxy-4-methyl-3-pyridin-4-yl-chromen-2-one | HCID 11659018 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 7-Hydroxy-4-methyl-3-pyridin-4-yl-chromen-2-one | HCID 135502913 | — |
反応手順
To a solution of 7-methoxy-4-methyl-3-pyridin-4-yl-chromen-2-one (600 mg, 2.24 mmoL) in CH2Cl2 (10 mL) at 0° C. was added EtSH (˜1 mL) followed by AlBr3 (6.74 mmoL, 1.80 g). The mixture was slowly warm to room temperature and poured into ice sat. NaHCO3 solution. Extraction was conducted 3× with CH2Cl2. The combined organic layer was washed with brine, dried over anhydrous Na2SO4, filtered and concentrated to give the crude material, which was then purified by silica gel column chromatography using hexanes:ethyl acetate 1:1 as eluent to afford the title product as pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07399767B2 |
| 出典データセット | uspto-grants-2008_07 |
| ORD ID | ord-2f8b5397725240e8bf29bd29c8541eb3 |
| 出典メモ | uspto-grants-2008_07 |