化工社化工社 化学情報印刷レポート · 研究参考用
Acetic Acid → 1,3-Benzenediol,5-[5-(trifluoromethyl)-2-benzothiazolyl]-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 2-Amino-4-(trifluoromethyl)benzenethiol | HCID 88042 | — |
| 反応物 | 3,5-Dihydroxybenzaldehyde | HCID 94365 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1,3-Benzenediol,5-[5-(trifluoromethyl)-2-benzothiazolyl]- | HCID 60194580 | 37% |
反応手順
In an acetic acid (0.42 mL) solvent, a mixture including 2-amino-4-(trifluoromethyl)benzenethiol (100 mg, 0.44 mmol), 3,5-dihydroxybenzaldehyde (60 mg, 0.44 mmol), and sodium acetate (107 mg, 1.30 mmol) was refluxed for 6.5 hours. After cooling, the reaction mixture was distributed between ethyl acetate and water, and an organic layer was dried by using MgSO4, filtered, and evaporated under reduced pressure. The residual was purified by silica gel column chromatography using hexane and ethyl acetate (2:1) as a developer to obtain a solid Compound 36 (50.6 mg, 37%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08889881B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-108a4233051447f7bc04b01daefe397e |
| 出典メモ | uspto-grants-2014_11 |