化工社化工社 化学情報印刷レポート · 研究参考用
Water → Methyl 2-(4-bromothiophen-2-yl)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Methyl thiophen-2-acetate | HCID 88055 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | Methyl 2-(4-bromothiophen-2-yl)acetate | HCID 67367159 | 41.2% |
反応手順
To a solution of methyl 2-(thiophen-2-yl)acetate (5 g, 32 m mol) and anhydrous AlCl3 (10.7 g, 80 mmol) in CHCl3 (50 ml) was added dropwise bromine (1.8 ml, 34 mmol) at 0˜5° C. over 30 min. When the addition was complete, the mixture was allowed to warm to room temperature overnight. Then it was poured into icy water (50 ml), extracted with EtOAc (30 ml×3). The combined organic phase was dried over Na2SO4, filtered and concentrated. Purification by column chromatography (PE/EtOAc=10/1) gave the product (3.1 g, 41%) as light yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09187447B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-c684f8a700ae4cda99395bea95117d31 |
| 出典メモ | uspto-grants-2015_11 |