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Tetrahydrofuran → 4-Octyloxy-benzoic acid 4-(4-hydroxy-cyclohexyl)-phenyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Diisopropylcarbodiimide | HCID 12734 | — |
| 反応物 | 4-(Octyloxy)benzoic acid | HCID 17231 | — |
| 反応物 | Methyl 2-hydroxy-4-octyloxybenzoate | HCID 11536459 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 生成物 | 4-Octyloxy-benzoic acid 4-(4-hydroxy-cyclohexyl)-phenyl ester | HCID 69307345 | 27% |
反応手順
10 g (0.052 mol) of 4-(4-Hydroxy-cyclohexyl)-phenol obtained in Step 1 of the synthesis of the compound 27 and 13.02 g (0.052 mol) of 4-Octyloxy-benzoic acid are dissolved in 120 mL of anhydrous THF. 0.65 g (0.0052 mol) of DMAP, then 6.56 g (0.052 mol) of DIC are added. The mixture is stirred at room temperature overnight. The solvent is distilled off and then the resulting product is purified by column chromatography on silica gel using mixture of hexane and ethyl acetate (70:30) as eluent and recrystallised from ethanol to give a pure product as a white solid (6 g, 27% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07416682B2 |
| 出典データセット | uspto-grants-2008_08 |
| ORD ID | ord-6785549646bf4f4087b04dfa766f68f1 |
| 出典メモ | uspto-grants-2008_08 |