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tert-Butanol → (4-Phenyl-but-3-ynyl)-carbamic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | tert-Butanol | HCID 6386 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| 反応物 | 5-phenylpent-4-ynoic Acid | HCID 10975983 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (4-Phenyl-but-3-ynyl)-carbamic acid tert-butyl ester | HCID 23544319 | — |
反応手順
A solution of 5-phenylpent-4-ynoic acid (0.49 g), diphenylphosphoryl azide (0.66 mL) and triethylamine (0.43 mL) was refluxed in 15 mL toluene for 3 h. The reaction was cooled to rt and t-butyl alcohol was added. The reaction was refluxed for 16 h, then the volatile materials were removed via a rotary evaporator. The residue was purified by column chromatography on silica (2–6% ethyl acetate in hexanes) to give (4-phenyl-but-3-ynyl)-carbamic acid tert-butyl ester (0.3 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07084154B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-5939bb060647439fbc9218ef92c27765 |
| 出典メモ | uspto-grants-2006_08 |