関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl chlorophosphate | HCID 13139 | — |
| 反応物 | 2-tert-Butyl-4-methylphenol | HCID 17004 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Tert-butyl-4-methylphenyl diethyl phosphate | HCID 59129394 | 100% |
反応手順
To a suspension of NaH (60% in mineral oil, 8.4 g, 0.21 mol) in THF (200 mL) was added dropwise a solution of 2-tert-butyl-4-methylphenol (33 g, 0.20 mol) in THF (100 mL) at 0° C. The mixture was stirred at 0° C. for 15 min and then phosphorochloridic acid diethyl ester (37 g, 0.21 mol) was added dropwise at 0° C. After addition, the mixture was stirred at ambient temperature for 30 min. The reaction was quenched with sat. NH4Cl (300 mL) and then extracted with Et2O (350 mL×2). The combined organic layers were washed with brine, dried over anhydrous Na2SO4, and then evaporated under vacuum to give 2-tert-butyl-4-methylphenyl diethyl phosphate (contaminated with mineral oil) as a colorless oil (60 g, ˜100%), which was used directly in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07776905B2 |
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| 出典データセット | uspto-grants-2010_08 |
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| ORD ID | ord-1cceac48c1db4e91ae64754c79377175 |
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| 出典メモ | uspto-grants-2010_08 |
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