化工社化工社 化学情報印刷レポート · 研究参考用
1-Fluoro-4-hydroxy-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate) → 5-Tert-butyl-2-fluoro-indan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Fluoro-4-hydroxy-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate) | HCID 2737329 | — |
| 反応物 | 5-Tert-butyl-2,3-dihydroinden-1-one | HCID 11030576 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-Tert-butyl-2-fluoro-indan-1-one | HCID 67188230 | — |
反応手順
5-tert-butyl-indan-1-one (7.53 g, 40 mmol) was dissolved in methanol (400 ml). Accufluor (32.18 g) was added, and the reaction heated to reflux for 2 hours. After cooling and removing the solvent under vacuum, the residue was taken in methylene chloride and filtered. The filtrate was washed with water, dried with magnesium sulfate, and filtered, and the solvent removed under vacuum to give 5-tert-Butyl-2-fluoro-indan-1-one, which was used without further purification. 1H NMR (300 MHz, CDCl3) 7.73 (d, 1H), 7.48 (d, 1H), 7.45 (s, 1H), 5.18-5.35 (m, 1H), 3.54-3.65 (m, 1H), 3.12-3.29 (m, 1H), 1.36 (s, 9H). MS (CSI) m/e 224 (M+NH4)+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08487116B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-4b0788c3764f40829af90ba225641ad4 |
| 出典メモ | uspto-grants-2013_07 |