참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylamine | HCID 674 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Hydrazinecarboxylic acid, ethyl ester | HCID 20064 | — |
| 반응물 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 반응물 | [Chloro(dimethylamino)methylidene]-dimethylazanium chloride | HCID 177416803 | — |
| 용매 | Phenol | HCID 996 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-amino-5-dimethylamino-2,4-dihydro-3H-1,2,4-triazol-3-one | HCID 15116960 | — |
반응 단계
A mixture of 104 g (1 mol) of ethyl hydrazinoformate, 200 g of phenol, 50 ml of dimethyl formamide and 106 g (1 mol) of sodium carbonate is initially introduced under a water-jet vacuum and a solution of 171 g (1 mol) of tetramethylchloroformamidinium chloride in 200 g of phenol is added in such a manner that a temperature of 40° C. is not exceeded, water being gradually distilled off. Then the mixture is heated slowly, 55 g (1.1 mol) of hydrazine hydrate are added at 80° C. and the mixture is heated under atomspheric pressure in the course of 3 hours until phenol is refluxed (at about 190° C.), dimethylamine being eliminated. The phenol is then distilled off under a water-jet vacuum, the residue is treated with 750 ml of (hot) ethoxyethanol, the salt is separated off by filtration under heat and the filtrate is cooled. The crystalline product obtained in this manner is isolated by suction filtration. 49g (34% of theory) of 4-amino-5-dimethylamino-2,4-dihydro-3H-1,2,4-triazol-3-one of melting point 205° C. are obtained. ##STR350##
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05220032 |
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| 출처 데이터셋 | uspto-grants-1993_06 |
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| ORD ID | ord-65ade8ffe8f744d3a142052f0ca63e86 |
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| 출처 메모 | uspto-grants-1993_06 |
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