関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Nitrophenol | HCID 980 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Isopropyl chloroformate | HCID 7917 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Nitrophenyl isopropyl carbonate | HCID 23390373 | — |
反応手順
Into a solution of 3.00 g of 4-nitrophenol and 3.31 mL of triethylamine in 30 mL of tetrahydrofuran, 2.46 mL of isopropyl chloroformate was dropped under cooling on ice. To the reaction mixture, after stirred at the same temperature for 10 min, ethyl acetate and water were added. The organic layer was separated, washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate, followed by solvent removal by evaporation under reduced pressure. The residue was dissolved in 50 mL of ethyl acetate, washed with a 5% potassium carbonate aqueous solution and a saturated sodium chloride aqueous solution successively and dried over anhydrous magnesium sulfate. After removing the solvent by evaporation under reduced pressure, 3.00 g of 4-nitrophenyl isopropyl carbonate was obtained as a light yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536343B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-cc3e370ad82d4fa1bf0fa21ad081678d |
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| 出典メモ | uspto-grants-2013_09 |
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