関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6-Chloro-[1,2,4]triazolo[4,3-b]pyridazine | HCID 313624 | — |
| 反応物 | 4-Benzhydryl-1-piperazinepropanol | HCID 15524146 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-[3-[4-(Diphenylmethyl)-1-piperazinyl]propoxy][1,2,4]triazolo[4,3-b]pyridazine | HCID 15524147 | 79% |
反応手順
0.311 g of 4-(diphenylmethyl)-1-piperazinepropanol was dissolved in 5 ml of N,N-dimethylformamide; 0.048 g of 60% oily sodium hydride was added; the reaction mixture was stirred in an oil bath (60° C.) for 30 minutes. After cooling, 0.232 g of 6-chloro[1,2,4]triazolo[4,3-b]pyridazine was added; the reaction mixture was stirred in an oil bath. (bath temperature 60° C.) for 40 minutes. After cooling, ice water was added; the reaction mixture was extracted with ethyl acetate; the extract was washed with saline and dried over magnesium sulfate. After concentration under reduced pressure, the residue was subjected to silica gel column chromatography and eluted with ethyl acetate-methanol-triethylamine (90:10:1). The desired fraction was collected and concentrated; the crystal obtained was filtered, washed with ethyl ether, and dried, to yield 0.339 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06610694B1 |
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| 出典データセット | uspto-grants-2003_08 |
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| ORD ID | ord-fd7000f227e04a6cbe60a298e7d815b0 |
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| 出典メモ | uspto-grants-2003_08 |
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