関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzoic acid, 4-fluoro-, ethyl ester | HCID 67976 | — |
| 反応物 | Dimethylpiperazine | HCID 198037 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | Ethyl 4-(3,4-dimethylpiperazin-1-yl)benzoate | HCID 57440404 | 36.2% |
反応手順
1,2-Dimethyl-piperazine (0.914 g, 8.00 mmol) and ethyl 4-fluorobenzoate (0.587 mL, 4 mmol) were dissolved in DMA (6 mL) and sealed into a microwave tube. The reaction was heated to 150° C. for 90 mins in the microwave reactor and cooled to room temperature. The reaction mixture was evaporated and the crude product was purified by silica column chromatography, eluting with 5% MeOH in DCM (containing 0.1% 0.880 ammonia). Pure fractions were evaporated to dryness to afford ethyl 4-(3,4-dimethylpiperazin-1-yl)benzoate (0.380 g, 36.2%) as a colourless waxy solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07737149B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-b9499f38f1d64c97b53dac0a329dbab8 |
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| 出典メモ | uspto-grants-2010_06 |
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