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Potassium Phosphate, Dibasic → 2-(4-Fluoro-3-methylphenyl)-4,4,6,6-tetramethyl-1-epoxycyclohexane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Phosphate, Dibasic | HCID 24450 | — |
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | 4'-Fluoro-3,3,3',5,5-pentamethyl-2,3,4,5-tetrahydro-1,1'-biphenyl | HCID 2769351 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(4-Fluoro-3-methylphenyl)-4,4,6,6-tetramethyl-1-epoxycyclohexane | HCID 53934303 | 88% |
反応手順
A solution of meta-chloroperbenzoic acid (20 g, 90 mmol) in 250 ml of CH2Cl2 is added dropwise to a cooled (0° C.) solution of 1-fluoro-2-methyl-4-(3,3,5,5-tetramethylcyclohex-1-en-1-yl)benzene (15 g, 61 mmol) and K2HPO4 (21 g, 90 mmol) in dry CH2Cl2 (100 ml). The resulting milky solution is stirred at room temperature for 14 hours, filtered and washed successively with 5% cold NaOH (2×50 ml), H2O (2×50 ml) and brine (75 ml). The CH2Cl2 fraction is dried (MgSO4), and the solvent is removed under reduced pressure to provide 14 g (88%) of 2-(4-fluoro-3-methylphenyl)-4,4,6,6-tetramethyl-1-epoxycyclohexane: 1H NMR δ=0.9 (s,6), 0.95 (s,3), 1.1 (s,3), 1.15 (q,2), 1.85 (AB-q, 2), 2.1 (s,3), 2.55 (s,1), 6.85 (t,1), 7.1 (t,1), 7.25 (dd,1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05248830 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-6f275656c8da41b3801c8b460fc918fa |
| 出典メモ | uspto-grants-1993_09 |