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Sodium Hydroxide → 2-(3,5-Diphenyl-pyrazol-1-yl)-1-(4-(2-pyrimidinyl)-1-piperazinyl)-ethanon
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1-(2-Pyrimidinyl)piperazine | HCID 88747 | — |
| 反応物 | (3,5-Diphenyl-pyrazol-1-yl)-acetic acid | HCID 824607 | — |
| 反応物 | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(3,5-Diphenyl-pyrazol-1-yl)-1-(4-(2-pyrimidinyl)-1-piperazinyl)-ethanon | HCID 86762672 | 73.1% |
反応手順
278 mg (3,5-diphenyl-pyrazol-1-yl)-acetic acid was dissolved in 5 mL DMF. 321 mg TBTU and 172 μL DIPEA were added to this solution and the mixture was stirred for a few minutes at RT. 164 mg 2-(1-piperazinyl)-pyrimidine was added and stiffing was continued for 30 min. Then 10 mL of a 1M NaOH solution and 50 mL CH2Cl2 were added, the organic phase was separated. The solvent was removed and the residue was purified by flash chromatography (silica gel, DCM/MeOH/NH3 0-5%). Diethylether was given to the residue and the precipitate was filtered to yield 310 mg of the desired compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822464B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-49b5a83dc13b4d57b96ba0b47e36f155 |
| 出典メモ | uspto-grants-2014_09 |