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Ethyl Acetate → [4-(Methanesulfonylaminocarbonyl)butyl]triphenylphosphonium bromide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 5-Bromo-N-methanesulfonylpentanamide | HCID 20296141 | — |
| 反応物 | Ethylacetate acetone | HCID 21584569 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | [4-(Methanesulfonylaminocarbonyl)butyl]triphenylphosphonium bromide | HCID 19608840 | 78% |
反応手順
A stirring mixture consisting of triphenylphosphine (13.2 g, 24.4 mmol) and 5-bromo-N-(methylsulfonyl)pentanamide (prepared in Step A, 5.55 g, 21.5 mmol) in xylene (15 mL) was brought to reflux for 4 hours. Subsequently, ethyl acetate was added to the hot reaction mixture and stirring was continued for the next 15 minutes. The crude product was isolated from acetone-ethyl acetate to afford the title intermediate (8.68 g, 78%); melting point 189-190° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08063240B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-62de46e6eef545028d030342528bad0f |
| 出典メモ | uspto-grants-2011_11 |