関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-chloro-N,N-dimethylacetamide | HCID 75886 | — |
| 反応物 | 4-(6-(4-Isopropylpiperazin-1-yl)-pyridazin-3-yl)-phenol | HCID 136099409 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 131730788 | HCID 131730788 | — |
反応手順
A mixture of 4-[6-(4-isopropyl-piperazin-1-yl)-pyridazin-3-yl]-phenol (110 mg, 0.37 mmol) and 60% sodium hydride (58 mg, 1.45 mmol) in dry DMF (5 mL) was heated at 60° C. for 30 min. 2-Chloro-N,N-dimethylacetamide (54 mg, 0.44 mmol) was added and heating at 60° C. was continued for another 20 h. The reaction mixture was evaporated to dryness and partitioned between water (10 mL) and DCM (10 mL). The organic phase was isolated, washed with brine (5 mL), dried over anhydrous magnesium sulphate, and evaporated to dryness in vacuo. The residue was dissolved in hot ethyl acetate and HClg in Et2O was added to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846677B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-ad58286448e340c4add39b118395f36f |
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| 出典メモ | uspto-grants-2014_09 |
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