化工社化工社 化学情報印刷レポート · 研究参考用
Toluene → HCID 22285400、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Bromomethylcyclopropane | HCID 81503 | — |
| 反応物 | Ethyl 1,3-dithiane-2-carboxylate | HCID 88552 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 22285400 | HCID 22285400 | — |
反応手順
To a flamed dried flask is added dry toluene (80 mL) and sodium hydride (60%, 33.5 mmol, 1.34 g). The reaction is cooled in a ice bath and a solution of ethyl 1,3 dithiane carboxylate (52 mmol, 10 g) and bromomethyl cyclopropane (62.4 mmol, 8.42 g) in DMF (24 mL) are added dropwise over 10 minutes. The ice bath is removed and the reaction is stirred for 18 h. Water is added (50 mL) and the organic layer is separated. The organic layer is washed with brine, dried (Na2SO4), and concentrated to a yellow oil (12 g, 92%). LC-ES/MS: 247.0 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08153624B2 |
| 出典データセット | uspto-grants-2012_04 |
| ORD ID | ord-2b7089650b25413781be88d029022323 |
| 出典メモ | uspto-grants-2012_04 |