関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Methyl bromoacetate | HCID 60984 | — |
| 反応物 | Phosphonium, (2-methoxy-2-oxoethyl)triphenyl-, bromide (1:1) | HCID 2733211 | — |
| 反応物 | Phosphonium | HCID 5460504 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Acetic acid, 2-(triphenylphosphoranylidene)-, methyl ester | HCID 17453 | 80% |
反応手順
Triphenyl phosphine (13 g.) was dissolved in dry benzene (60 ml.) and methyl bromoacetate (8.3 g.) was added dropwise. The solution was heated at 70° C., for 2 days, and then cooled and filtered. The residue was washed with benzene and dried to give about 16 g. of (methoxycarbonyl methyl)triphenylphosphonium bromide. The phosphonium salt (10 g.) was dissolved in water (250 ml.) and 5% aqueous sodium hydroxide was added dropwise with stirring until the solution became alkaline to litmus. The resulting precipitate was filtered off, washed with water and dried. Crystallisation from ethyl acetate/petroleum spirit gave (methoxycarbonyl methylene) triphenyl phosphorane as a colourless solid in about 80% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05004822 |
|---|
| 出典データセット | uspto-grants-1991_04 |
|---|
| ORD ID | ord-9ef48c9e50854c13b908506907206612 |
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| 出典メモ | uspto-grants-1991_04 |
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