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Sodium Bicarbonate → 6-[3-[4-(Diphenylmethoxy)piperidino]-2-hydroxypropylamino][1,2,4]triazolo[1,5-b]pyridazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 6-Chloro-(1,2,4)triazolo(1,5-b)pyridazine | HCID 11240611 | — |
| 反応物 | 3-[4-(Diphenylmethoxy)piperidino]-2-hydroxypropylamine | HCID 22989280 | — |
| 生成物 | 6-[3-[4-(Diphenylmethoxy)piperidino]-2-hydroxypropylamino][1,2,4]triazolo[1,5-b]pyridazine | HCID 22989428 | 56% |
反応手順
0.675 g of 3-[4-(diphenylmethoxy)piperidino]-2-hydroxypropylamine and 0.335 g of 6-chloro[1,2,4]triazolo [1,5-b]pyridazine were stirred at 135-140° C. for 3 hours. After cooling, aqueous sodium bicarbonate was added, followed by extraction with ethyl acetate-tetrahydrofuran (2:1); the extract was washed with saline and dried with sodium sulfate. The dry product was concentrated 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, recrystallized from ethyl acetate and dried to yield 0.509 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06248740B1 |
| 出典データセット | uspto-grants-2001_06 |
| ORD ID | ord-134a977e4c4e49b18d1d70faa17616d6 |
| 出典メモ | uspto-grants-2001_06 |