関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Methallyl alcohol | HCID 10557 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 4-Nitrophenyl chloroformate | HCID 82129 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Carbonic acid 2-methylallyl ester 4-nitrophenyl ester | HCID 67469869 | — |
反応手順
Methallyl alcohol [CAS No. 513-42-8] (5 g) and 4-nitrophenyl chloroformate [CAS No. 7693-46-1] (12.6 g) were dissolved in THF (70 mL), and pyridine (6.69 mL) was added to the resulting mixture under ice-cooling, after which the resulting mixture was stirred overnight at room temperature. To the reaction mixture, ice and saturated aqueous ammonium chloride solution were added, and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. The resulting mixture was filtered, and the filtrate obtained was concentrated under reduced pressure. The residue obtained was purified by silica gel column chromatography (mixed solvent of heptane-ethyl acetate) to obtain the captioned compound (10.5 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08436009B2 |
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| 出典データセット | uspto-grants-2013_05 |
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| ORD ID | ord-b0bc7230f5da40cc88c91493b35446c3 |
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| 出典メモ | uspto-grants-2013_05 |
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