化工社化工社 化学情報印刷レポート · 研究参考用
Formaldehyde → HCID 68865887、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | (Z)-3-((1H-pyrrol-2-yl)methylene)indolin-2-one | HCID 5908088 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | HCID 68865887 | HCID 68865887 | 50% |
反応手順
A mixture of Z-(1H-Pyrrol-2-ylmethylene)-1,3-dihydro-indol-2-one (120 mg, 0.57 mmol), paraformaldehyde (32 mg, 1.1 mmol), and morpholine (62.2 μL, 0.71 mmol) in 8.0 mL of 20% dioxane in EtOH was heated at reflux for 19.5 h. The reaction mixture was concentrated and paraformaldehyde (10.0 mg, 0.33 mmol), morpholine (15 μL, 0.17 mmol) and EtOH (7 mL) was added. The reaction mixture refluxed for 24 h. The reaction mixture was cooled to room temperature and concentrated. The residue was dissolved in 15 mL of CHCl3 and treated with activated charcoal. The resulting suspension was filtered and the filtrate concentrated. The residue was crystallization from ethyl acetate/hexane to give the title compound (88.0 mg, 50%) as a bright yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06699863B1 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-7796d9be31304c5281081c9b2e12dd9e |
| 出典メモ | uspto-grants-2004_03 |