化工社化工社 化学情報印刷レポート · 研究参考用
1,3-Dibromopropane → 9-chloro-3,4-dihydro-2H-1,5-benzodioxepine-7-carbaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,3-Dibromopropane | HCID 8001 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Chloro-4,5-dihydroxybenzaldehyde | HCID 2468182 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 9-chloro-3,4-dihydro-2H-1,5-benzodioxepine-7-carbaldehyde | HCID 4962246 | — |
反応手順
A mixture of 3-chloro-4,5-dihydroxy benzaldehyde (4.15 g), of 1,3-dibromopropane (4.71 g, 0.92 eq.) and potassium carbonate (8.28 g, 2.5 eq.) in acetonitrile (160 ml) was heated to 60° C. overnight. The mixture was allowed to cool to room temperature and filtered. The filtrate was concentrated under reduced pressure. The residue was purified by flash chromatography on silica (20% ethyl acetate in hexanes) to give the product as a white crystal. MS (m+1)=212.1
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08722896B2 |
| 出典データセット | uspto-grants-2014_05 |
| ORD ID | ord-5ea4580f0c9f4e5a95641458ceba33f3 |
| 出典メモ | uspto-grants-2014_05 |