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Sodium hydride → Bis(4-trifluoromethylthiobenzyl)ether
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-((Trifluoromethyl)thio)benzenemethanol | HCID 2777870 | — |
| 反応物 | 4-(Trifluoromethylthio)benzyl bromide | HCID 2777882 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Bis(4-trifluoromethylthiobenzyl)ether | HCID 12112481 | 87.2% |
反応手順
Sodium hydride (65 mg 60% dispersion oil, 1.58 mmol) was added to a solution of 4-(trifluoromethylthio)benzyl alcohol (300 mg, 1.44 mmol) in THF (10 mL) at rt. After stirring for 10 min, to the mixture was added 4-(trifluoromethylthio)benzyl bromide (410 mg, 1.51 mmol), stirring was continued overnight. The reaction was quenched with saturated ammonium chloride solution, extracted with EtOAc, washed with water and dried to give 0.5 g (85%) of bis(4-trifluoromethylthiobenzyl) ether as a yellow oil. 1HNMR (360 MHz, DMSO-d6) δ 7.70 (d, J=8.1 Hz, 4H), 7.53 (d, J=8.1 Hz, 4H), 4.65 (s, 4H, CH2OCH2). MS-EI m/z 398 [M+].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06596772B1 |
| 出典データセット | uspto-grants-2003_07 |
| ORD ID | ord-b6758ded59d74e05aee992c35e218b2b |
| 出典メモ | uspto-grants-2003_07 |