関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Cyclohexylresorcinol | HCID 75055 | — |
| 反応物 | (Chloro(phenylmethoxy)phosphoryl)oxymethylbenzene | HCID 4641201 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 86682691 | HCID 86682691 | 64% |
反応手順
To a tetrahydrofuran solution (10 ml) of 4-cyclohexylresorcinol (926 mg), sodium hydride (60% dispersion in liquid paraffin) (404 mg) was added and stirred at 0° C. for 30 minutes. Then, dibenzyl chlorophosphate (10 w/v % solution in benzene) (30 ml) was added dropwise. After stirring at room temperature for 3 hours, water (30 ml) was added to the reaction mixture, and the extraction was carried out with ethyl acetate (30 ml). Then, the extract was washed with saturated brine (20 ml), dried with anhydrous sodium sulfate and then concentrated. The residue (4.12 g) was subjected to silica gel chromatography (silica gel 90 g, chloroform to chloroform:methanol=100:1), to give 1,3-bis(dibenzylphosphonooxy)-4-cyclohexylbenzene (2.19 g, yield: 64%) as a yellow liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08486919B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-e3fe8978e03448e5b19ee71f2e107697 |
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| 出典メモ | uspto-grants-2013_07 |
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