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Triphenylphosphine → 2-(Prop-1-yn-1-yl)benzene-1-sulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Dipivefrin Hydrochloride | HCID 71486 | — |
| 反応物 | 2-Iodobenzene-1-sulfonamide | HCID 2824892 | — |
| 触媒 | Palladium Chloride | HCID 24290 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 2-(Prop-1-yn-1-yl)benzene-1-sulfonamide | HCID 19793610 | 80% |
反応手順
To a solution of 28.3 g (0.1 mole) of 2-iodophenylsulfonamide in 350 ml of dimethylformamide and 100 ml of triethylamine are added 1.0 g of palladium dichloro-bis(triphenylphosphite) complex, PdCl2 [P(C6H5)3 ]2, and 0.5 g of copper (I) iodide (CuI). Gaseous propine is then introduced into this solution until the starting material is completely reacted. The reaction mixture is filtered and the residue is concentrated in vacuo and then taken up in water. The precipitate is isolated and dried. Recrystallisation from ethyl acetate/hexane yields 15.6 g (80%) of 2-(propyn-1-yl)phenylsulfonamide with a melting point of 147°-149° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04537618 |
| 出典データセット | uspto-grants-1985_08 |
| ORD ID | ord-5057f5566bbc4f45a1d58d017f72023f |
| 出典メモ | uspto-grants-1985_08 |