関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Tetraisopropyl methylenediphosphonate | HCID 74266 | — |
| 反応物 | 2-Bromoethyl trityl ether | HCID 10959531 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1,1-Bis(diisopropoxyphosphinoyl)-3-triphenylmethoxypropane | HCID 21841998 | 77.4% |
反応手順
Under a nitrogen atmosphere, 60% sodium hydride (200 mg), 1-bromo-2-triphenylmethoxyethane (1.84 g) and tetraisopropyl methylenebisphosphonate (1.72 g) were suspended in toluene (5 ml), and the resulting suspension was stirred at 120° C. for 7 hours. The reaction mixture was diluted with toluene, and then a saturated aqueous ammonium chloride solution was added thereto to decompose the excess sodium hydride. Then, ethyl acetate was added thereto to effect separation, and the organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by a silica gel column chromatography (chloroform:acetone) to obtain 1,1-bis(diisopropoxyphosphinoyl)-3-triphenylmethoxypropane (2.44 g, yield 77%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05962438 |
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| 出典データセット | uspto-grants-1999_10 |
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| ORD ID | ord-3d253bd6539e4ec89bb0faf99b9f6fb4 |
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| 出典メモ | uspto-grants-1999_10 |
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