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Tert-Butylamine → 4-Decyloxycarbonyl-4'-hydroxybiphenyl
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tert-Butylamine | HCID 6385 | — |
| 反応物 | 1-Decanol | HCID 8174 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 2-Dimethylaminopyridine | HCID 21885 | — |
| 反応物 | 4'-Acetoxy-biphenyl-4-carboxylic acid | HCID 611836 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Decyloxycarbonyl-4'-hydroxybiphenyl | HCID 14847575 | 64.2% |
反応手順
To a solution of n-decanol (1.6 g) and 4-methylcarbonyloxy-4'-carboxybiphenyl (2.6 g) in tetrahydrofuran (50 ml) were added dicyclohexylcarbodiimide (1.4 g) and dimethylaminopyridine (0.5 g), followed by stirring at room temperature for 24 hours. Thereto was added tert-butylamine and the mixture was refluxed at 70° C. for 2 hours and hydrolyzed. After the solvent was distilled off, dilute hydrochloric acid was added to make the solution neutral and the solution was extracted with diethyl ether. After the solvent was distilled off, the residue was washed with hexane and recrystallized from water/ethanol (1/9) solution to obtain the titled compound (about 2.3 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05891359 |
| 出典データセット | uspto-grants-1999_04 |
| ORD ID | ord-e60debf559bd49ddaf67dcd77e170b49 |
| 出典メモ | uspto-grants-1999_04 |