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Ammonium Chloride → 2-{4-[2-(3,5-Dimethyl-pyrazol-1-yl)-acetyl]-piperazin-1-yl}-benzoic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | (3,5-Dimethyl-1H-pyrazol-1-yl)acetic acid | HCID 572875 | — |
| 反応物 | Bis-(1H-imidazol-2-YL)-methanone | HCID 5250894 | — |
| 反応物 | Methyl 2-(piperazin-1-yl)benzoate | HCID 10932975 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-{4-[2-(3,5-Dimethyl-pyrazol-1-yl)-acetyl]-piperazin-1-yl}-benzoic acid methyl ester | HCID 66599729 | 85.7% |
反応手順
To a vial containing the 2-piperazin-1-yl-benzoic acid methyl ester (0.667 g, 3.03 mmol) is added a pre-mixed solution containing (3,5-dimethyl-pyrazol-1-yl)-acetic acid (0.428 g, 2.78 mmol) and carbonyl diimidazole (0.567 g, 3.50 mmol). The mixture is stirred overnight and then diluted with 200 mL of EtOAc followed by 200 mL of sat. NH4Cl. The organic phase is washed with 2×200 mL of H2O and 1×200 mL of brine. The organic phase is dried with MgSO4, filtered and concentrated to give 0.849 g of 2-{4-[2-(3,5-dimethyl-pyrazol-1-yl)-acetyl]-piperazin-1-yl}-benzoic acid methyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08450317B2 |
| 出典データセット | uspto-grants-2013_05 |
| ORD ID | ord-e0d41b05ed414d209f28cc350e1aac4f |
| 出典メモ | uspto-grants-2013_05 |