関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloromethyl Methyl Ether | HCID 7864 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Propyl-4-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)phenylacetate | HCID 86639401 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(1,1,1,3,3,3-Hexafluoro-2-(methoxymethoxy)propan-2-yl)-2-propylphenol | HCID 59201037 | 79% |
反応手順
2-Propyl-4-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)phenylacetate (13.67 g, 39.7 mmol) in dichloromethane (160 mL) was added with N,N-diisopropylethylamine (27.6 mL) and then with chloromethyl methyl ether (6.0 mL). The resultant mixture was stirred at 40° C. for 18 hours, added with methanol at room temperature (20 mL), stirred for 1.5 hours, then added with potassium carbonate (11 g, 39.7 mmol), and stirred overnight. The reaction solution was added with water and extracted with ethyl acetate. The organic layer was washed with brine, dried using anhydrous sodium sulfate, and concentrated in vacuo. The obtained residue was purified using silica-gel column chromatography (hexane/ethyl acetate) and the title compound (10.87 g, yield 79%) was obtained as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08153634B2 |
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| 出典データセット | uspto-grants-2012_04 |
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| ORD ID | ord-17e0dc7d6b3d4382a6b861997b29a704 |
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| 出典メモ | uspto-grants-2012_04 |
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