化工社化工社 化学情報印刷レポート · 研究参考用
Ethanol → Bis(4-n-pentylcyclohexylsulfonyl)diazomethane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | p-Toluenesulfonyl azide | HCID 13661 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Bis(4-n-pentylcyclohexylsulfonyl)methane | HCID 22737685 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Bis(4-n-pentylcyclohexylsulfonyl)diazomethane | HCID 22737629 | 46% |
反応手順
In 22.4 g of dimethylformamide were dissolved 22.5 g (0.050 mol) of the bis(4-n-pentylcyclohexylsulfonyl)methane prepared above and 14.8 g (0.075 mol) of p-toluenesulfonylazide. To this solution were added 90.1 g of ethanol and 22.2 g of water. The solution was cooled on an ice bath, to which 2.0 g (0.050 mol) of sodium hydroxide in 23 g of water was added dropwise at a temperature below 5° C. The solution was ripened at the temperature for 6.5 hours. Filtration of the crystals gave 2.6 g of the desired bis(4-n-pentylcyclohexylsulfonyl)diazomethane. The yield was 46%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06713612B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-7eaa13038eb44482a5d299dd3d4e07c0 |
| 出典メモ | uspto-grants-2004_03 |