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Water → Pyrinuron
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-Pyridinemethanamine | HCID 31018 | — |
| 反応物 | Carbamic acid, N-(4-nitrophenyl)-, methyl ester | HCID 74752 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | Pyrinuron | HCID 40813 | 88.2% |
反応手順
A mixture of 5.88 g (0.03 mole) of methyl N-(4-nitrophenyl)-carbamate, 2.70 g (0.025 mole) of 3-aminomethyl-pyridine, 9.6 ml of Gemanin CS 302D (a mixture of N,N-dimethyl-C10-18 alkylamines sold by the firm Hoechst AG) and 50 ml of xylene is filled into a flask equipped with a 20 cm Vigreux column and a Dean-Stark trap, and the mixture is boiled for 2 hours. During this period 6 ml of a mixture of water, methanol and xylene accumulate in the trap. The mixture is filtered when hot, the crystalline end-product is washed twice with 5 ml of hot xylene, each, and then with a few amount of acetone and dried. 6.0 g (88.2%) of N-(4-nitrophenyl)-N'-(3-pyridylmethyl)-urea are obtained; m.p.: 223°-225° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04410697 |
| 出典データセット | uspto-grants-1983_10 |
| ORD ID | ord-1f89c00beb094472a378de27ef9b1a5b |
| 出典メモ | uspto-grants-1983_10 |