関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzaldehyde | HCID 240 | — |
| 反応物 | Triphenyl phosphite | HCID 7540 | — |
| 反応物 | N,N-Dimethylsulfamide | HCID 134472 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | Diphenyl alpha-dimethylaminosulfonylaminobenzylphosphonate | HCID 21423543 | 36% |
反応手順
A mixture of 0.25 mole each of triphenyl phosphite, benzaldehyde, and N,N-dimethylsulfamide in 130g of chlorobenzene is warmed at 115° C. for 1.5 hrs. After the reaction mixture cools to room temperature, 41.0g (36% yield) of crude product is isolated by filtration. It is washed with water and recrystallized from chlorobenzene, giving a white solid: mp 193°-196°; 31P nmr (DMSO-d6) -14.0 ppm(d, J = 28Hz); 1H nmr δ8.8(d of d, 1, J = 2 and 11, NH), 6.8-7.8(m, 15, aryl), 5.2(d of d, 1, J = 10 and 25Hz, CH), 2.4(s, 6, CH3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04036913 |
|---|
| 出典データセット | uspto-grants-1977_07 |
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| ORD ID | ord-0d77e87ae00a4d888e672628fc48cff5 |
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| 出典メモ | uspto-grants-1977_07 |
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