関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Nefazodone | HCID 4449 | — |
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Benzene, (2-bromoethoxy)- | HCID 68526 | — |
| 反応物 | HCID 178437794 | HCID 178437794 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-phenoxyethyl-2H-1,2,4-triazol-3(4H)-one hydrochloride | HCID 136359214 | 53% |
反応手順
Reaction in Acetonitrile With Potassium Carbonate. A mixture of 2-[3-[4-(3-chlorophenyl)-1-piperazinyl]propyl]-5-ethyl-1H-1,2,4-triazol-3(2H)-one (15 g., 0.043 mole), phenoxyethyl bromide (8.62 g., 0.043 mole), potassium carbonate (11.9 g., 0.086 mole) and a trace of potassium iodide in 100 ml. of acetonitrile is refluxed for a 64 hr. period. The reaction mixture is filtered, the filtrate concentrated under reduced pressure and residual material taken up in ether and filtered. Concentration of the ethereal filtrate affords 18.35 g. (91%) of the free base product 2-[3-[4-(3-chlorophenyl)-1-piperazinyl]propyl]-5-ethyl-4-(2-phenoxyethyl)-2H-1,2,4-triazol-3(4H)-one. The free base is converted to the hydrochloride in ethanol employing ethanolic hydrogenchloride and crystallized from ethanol to afford a 53% yield of analytically pure 2-[3-[4-(3-chlorophenyl)-1-piperazinyl]propyl]-5 -ethyl-4-(2-phenoxyethyl-2H-1,2,4-triazol-3(4H)-one hydrochloride, m.p. 175°-177° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04575555 |
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| 出典データセット | uspto-grants-1986_03 |
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| ORD ID | ord-36ffb88d24914d9d91689d9ec5358028 |
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| 出典メモ | uspto-grants-1986_03 |
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