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 | 32.5% |
反応手順
1,2-Dimethylpiperazine (2.284 g, 20.00 mmol) and ethyl 4-fluorobenzoate (1.467 mL, 10 mmol) were dissolved in DMA (12 mL) and sealed in 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 heated for a further 30 mins at 150° C. 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 with 0.1% 0.880 ammonia. Pure fractions were evaporated to dryness to afford ethyl 4-(3,4-dimethylpiperazin-1-yl)benzoate (0.853 g, 32.5%) 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-5666ca763c844f3f9c153be3ed2cb867 |
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| 出典メモ | uspto-grants-2010_06 |
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