関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzene | HCID 241 | — |
| 反応物 | 4-Nitrobenzaldehyde | HCID 541 | — |
| 反応物 | Triphenyl phosphite | HCID 7540 | — |
| 反応物 | 1,1-Diphenylurea | HCID 33603 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | Diphenyl alpha-(3,3-diphenylureido)-4-nitrobenzylphosphonate | HCID 21423544 | — |
反応手順
A mixture of 21.2g (0.1 mole) of 1,1diphenylurea, 15.1g (0.1 mole) of 4-nitrobenzaldehyde, and 31.0g (0.1 mole) of triphenyl phosphite in 50g of benzene is stirred under nitrogen and warmed at reflux (87° C) for 2 hours to give a light yellow solution: 31P nmr -13.2 (d, J = 23Hz), 127.8 ppm (area ratio 5:1). Most of the benzene is removed at reduced pressure, and ether is stirred into the yellow oil remaining, causing 32g of solid to separate after a few minutes. A portion is recrystallized from acetonitrile to give a white solid: mp 157°-162°; 31P nmr -13.2 ppm (d, J = 24Hz); molecular weight (CHCl3) 565 (calcd 579).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04031170 |
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| 出典データセット | uspto-grants-1977_06 |
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| ORD ID | ord-f61df7b8542b466e981e5a526e84a0f1 |
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| 出典メモ | uspto-grants-1977_06 |
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