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Phenol → HCID 67333442、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenol | HCID 996 | — |
| 反応物 | 4-(Trifluoromethyl)cyclohexanone | HCID 2777491 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | HCID 67333442 | HCID 67333442 | — |
反応手順
A solution of 4-(trifluoromethyl)cyclohexanone (1.13 g, 6.8 mmol) and phenol (2.01 g, 21.4 mmol) in 3 mL of concentrated HCl (aq) was stirred at 40° C. for 18 h. The reaction mixture was diluted with EtOAc and saturated aqueous NaHCO3 was slowly added. The organic layer was collected and the aqueous layer was extracted twice with EtOAc. The combined organic layers were concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel eluting with a gradient of 0% to 40% EtOAc/hexanes over 10 column volumes, then 40% to 100% EtOAc/hexanes over 5 column volumes, affording the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07989472B2 |
| 出典データセット | uspto-grants-2011_08 |
| ORD ID | ord-66dcd8f751764dc8aef01be8a59c9e70 |
| 出典メモ | uspto-grants-2011_08 |