関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl chloroformate | HCID 6586 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-(Trifluoromethoxy)phenol | HCID 2777299 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 2-(trifluoromethoxy)phenyl carbonate | HCID 59395054 | 92% |
反応手順
2-(Trifluoromethoxy)phenol (6.0 g, 32.7 mmol) was dissolved in methylene chloride and triethylamine (9.1 mL, 65.4 mmol). The mixture was cooled to 0° C. and methyl chloroformate (2.8 mL, 36.0 mmol) was added dropwise. The mixture was stirred for 2 h at room temperature then quenched with saturated NH4Cl. The reaction was diluted with water and the aqueous layer extracted with dichloromethane (2×30 mL). The combined extracts were washed with water (100 mL) and brine (100 mL), dried over MgSO4, filtered and concentrated in vacuo to provide methyl 2-(trifluoromethoxy)phenyl carbonate (7.1 g, 92% yield). 1H NMR (400.0 MHz, DMSO-d6) δ7.36-7.26 (m, 4H), 3.93 (s, 31-1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08367660B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-e869c5241a46424dac7511930c5dd9c2 |
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| 出典メモ | uspto-grants-2013_02 |
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