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Dimethylformamide → 4-[1-(4-methoxyphenyl)-1H-indazol-3-yl]-1-piperazine carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Nitrourea | HCID 62372 | — |
| 反応物 | 1-(4-methoxyphenyl)-3-(1-piperazinyl)-1H-indazole hydrochloride | HCID 19887056 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-[1-(4-methoxyphenyl)-1H-indazol-3-yl]-1-piperazine carboxamide | HCID 15117116 | 85.4% |
反応手順
A solution of 1-(4-methoxyphenyl)-3-(1-piperazinyl)-1H-indazole hydrochloride (5.0 g, 0.01 mol), nitrourea (4.0 g, 0.04 mol) and dimethylformamide (200 ml) was warmed on a steam bath for 2 hours. The reaction mixture was poured into H2O and the aqueous mixture was extracted with ethyl acetate. The ethyl acetate was dried with MgSO4 and concentrated to 5.3 g of an oil. Crystallization was achieved with toluene affording 3.3 g (65%) of a powder. The powder was recrystallized again from toluene to afford 3.0 g of 4-[1-(4-methoxyphenyl)-1H-indazol-3-yl]-1-piperazine carboxamide, m.p. 155°-157° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04999356 |
| 出典データセット | uspto-grants-1991_03 |
| ORD ID | ord-7aee8f4086a642e3b79ffdea564f49a0 |
| 出典メモ | uspto-grants-1991_03 |