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Hydrochloric Acid → N-(2-Hydroxy-4-octyloxy-phenyl)-2,2,2-trifluoro-acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1-Bromooctane | HCID 8140 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | N-(2,4-dihydroxyphenyl)-2,2,2-trifluoro-acetamide | HCID 18454996 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(2-Hydroxy-4-octyloxy-phenyl)-2,2,2-trifluoro-acetamide | HCID 58685869 | 82.5% |
反応手順
To a solution of N-(2,4-dihydroxy phenyl)-2,2,2-trifluoro-acetamide (0.44 g; 2 mmol) in DMF (4 mL) was added K2CO3 and 1-bromooctane (0.37 mL; 2.1 mmol). The slurry was stirred for 2 days at room temperature, poured onto 0.1 M HCl (aq.; 50 mL) and then extracted with diethylether (30 mL). The organic phase was dried (MgSO4), filtered and the eluate evaporated to leave 550 mg of black solid which was purified by chromatography (SiO2; PE80-100° C./EtOAc=4:1) to leave 100 mg (15%) of a pure white solid. Mp. 114-116° C.; MS (GC-MS; Cl): 334 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741352B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-4ee9517eb9ec420cb4980422cdb446dd |
| 出典メモ | uspto-grants-2010_06 |