関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Methyl 4-(bromomethyl)benzoate | HCID 256687 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | [4-(Methoxycarbonyl)benzyl](triphenyl)phosphonium bromide | HCID 2764257 | 90.9% |
反応手順
To a 2 L 3-neck round bottom flask fitted with a glass stopper, rubber septum, and reflux condenser with a nitrogen inlet tube, was added 64.90 g (283 mmol) methyl 4-bromomethyl benzoate, 81.74 g (311 mmol) triphenylphosphine, and 744 mL toluene. The solution was heated at 80° C. for 5 h. After cooling to room temperature, the reaction vessel was placed in an ice bath. The resulting precipitate was filtered, washed with toluene, and dried in a vacuum oven to afford 126.35 g (89%) (4-carbomethoxy)benzyltriphenylphosphonium bromide as a white solid, mp.=248°-250° C.: 1H NMR (CDCl3, 200 MHz) d 3.86 (s, 3H), 5.70 (d, J=15.3 HZ, 2H), 7.24 (m, 4H), 7.71 (m, 15H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05243021 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-53a7d6a899654a0bba76c803935dd95c |
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| 出典メモ | uspto-grants-1993_09 |
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