関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Lauryldimethylamine | HCID 8168 | — |
| 反応物 | 3-Pyridinemethanamine | HCID 31018 | — |
| 反応物 | Carbamic acid, N-(4-nitrophenyl)-, methyl ester | HCID 74752 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | Pyrinuron | HCID 40813 | 80.3% |
反応手順
196.13 g (1 mole) of methyl N-(4-nitrophenyl)-carbamate, 108.14 g (1 mole) of 3-aminomethyl-pyridine and 106.7 g (0.5 mole) of N,N-dimethyl-n-dodecylamine are dissolved in 3 liters of xylene. The reaction mixture is refluxed, and the spures of water present are removed from the mixture together with the alcohol formed in a Dean-Stark trap. The end-product starts to separate from the mixture within 15-20 minutes from the beginning of boiling. The mixture is boiled for 4 hours, thereafter the suspension is filtered at about 100° to 110° C. The filter cake is washed twice with 100 ml of hot xylene, each, and with a small amount of acetone, and then dried in vacuo. 218.6 g (80.3%) of N-(4-nitrophenyl)-N'-(3-pyridylmethyl)-urea are obtained; m.p.: 221°-223° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04410697 |
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| 出典データセット | uspto-grants-1983_10 |
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| ORD ID | ord-d3de12e68bde4213939424b23bf92c4f |
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| 出典メモ | uspto-grants-1983_10 |
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