化工社化工社 化学情報印刷レポート · 研究参考用
Sodium hydride → 2-Chlorobenzenesulfonic acid 3-[5-cyanopentyloxy]-5-methylphenyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6-Bromohexanenitrile | HCID 81093 | — |
| 反応物 | 3-(2-Chlorophenylsulfonyloxy)-5-methylphenol | HCID 11277947 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Chlorobenzenesulfonic acid 3-[5-cyanopentyloxy]-5-methylphenyl ester | HCID 54033602 | 74.2% |
反応手順
Sodium hydride (24 mg, 1 mmol; 100%) was added to solution of 250 mg (0.855 mmol) of 2-chlorobenzenesulfonic acid 3-hydroxy-5-methylphenyl ester, as prepared in step (c) of Example 1, in 2 mL of N,N-dimethylformamide. After 5 min, 130 μL (0.93 mmol) of 6-bromohexanenitrile was added to the reaction mixture. The reaction mixture was stirred for 2 h at ambient temperature, quenched with brine (50 mL), extracted into diethyl ether (50 mL), washed with water (3×10 mL), dried (MgSO4), and concentrated in vacuo. The residue was purified by flash chromatography (methylene chloride/petroleum ether 4:1 to 100:0) to give 250 mg of the title compound as a colorless oil which solidified upon standing.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06281206B1 |
| 出典データセット | uspto-grants-2001_08 |
| ORD ID | ord-a32060e5af8244bdbee14082aca3e1e9 |
| 出典メモ | uspto-grants-2001_08 |