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Acetaldehyde → Phenyl [1-(p-tolylsulfonylamino)ethyl]phenylphosphinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetaldehyde | HCID 177 | — |
| 反応物 | P-Toluenesulfonamide | HCID 6269 | — |
| 反応物 | Diphenyl phenylphosphonite | HCID 239038 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | Phenyl [1-(p-tolylsulfonylamino)ethyl]phenylphosphinate | HCID 54172963 | 79% |
反応手順
A mixture of 0.15 mole each of diphenyl phenylphosphonite, acetaldehyde, and p-toluenesulfonamide in 100 g of chlorobenzene is stirred and warmed at 103°-115° C. for 1 hr, and the solvent and by-product phenol are removed by concentration of the reaction mixture to 120° at 0.5 mm. Ether is stirred into the residue, causing separation of 49.4g (79% yield) of solid product. Recrystallization twice from chlorobenzene gives a white solid: mp 178°-181°; 31P nmr (DMSO-d6)- 37.7 ppm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04032601 |
| 出典データセット | uspto-grants-1977_06 |
| ORD ID | ord-01c96d3c130a4e90a40e60e0bc6f3664 |
| 出典メモ | uspto-grants-1977_06 |