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Triphenylphosphine → [4-(Methanesulfonylaminocarbonyl)butyl]triphenylphosphonium bromide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 5-Bromo-N-methanesulfonylpentanamide | HCID 20296141 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | [4-(Methanesulfonylaminocarbonyl)butyl]triphenylphosphonium bromide | HCID 19608840 | 63.7% |
反応手順
A solution of 2.20 g. (8.57 mmoles) of the N-methanesulfonyl-5-bromovaleramide, prepared as above, 2.24 g. (8.57 mmoles) of triphenylphosphine, and 20 ml. of acetonitrile was heated to reflux under nitrogen overnight. The solution was then concentrated by rotary evaporation and the resultant solid was triturated with hot benzene (4X). The triturated solid was recrystallized from absolute ethanol:ether to afford the white, crystalline [4-(methanesulfonylaminocarbonyl)butyl]triphenylphosphonium bromide weighing 2.80 g. (63.7% yield) melting at 190°-191°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04087604 |
| 出典データセット | uspto-grants-1978_05 |
| ORD ID | ord-9611f217bbcd4502bb65382299ff236c |
| 出典メモ | uspto-grants-1978_05 |