化工社化工社 化学情報印刷レポート · 研究参考用
1,2-Dibromoethane → HCID 22646390、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dibromoethane | HCID 7839 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Hydroxycarbazole | HCID 104251 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 22646390 | HCID 22646390 | 32% |
反応手順
A mixture of 1.83 g (10 mmol) of 4-hydroxycarbazole (J. Chem. Soc. (1955), 3475-3477; J. Med. Chem. (1964) 7, 158-161), 1.08 ml (12,5 mmol) of 1,2-dibromoethane and 2.6 ml (10.5 mmol) of a 4 M aqueous solution of NaOH in 2 ml of water is heated under reflux for 5 hours. After the temperature returns to 20° C., the product is extracted using 2 times 30 ml of CH2Cl2. The organic solutions collected are then successively washed with 20 ml of water and 20 ml of salt water. After drying over MgSO4, filtration and concentration under vacuum, the residue is purified on a silica column (eluent: heptane/AcOEt: 80/20). A beige powder is obtained with a yield of 32%. Melting point: 135-136° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06809090B2 |
| 出典データセット | uspto-grants-2004_10 |
| ORD ID | ord-311e2387966e4a3692f8657e546c1282 |
| 出典メモ | uspto-grants-2004_10 |