関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Phenylpiperazine | HCID 7096 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 6-Chloro-5-formyl-1,3-dimethyluracil | HCID 319971 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 58484341 | HCID 58484341 | — |
反応手順
To an ice-cooled, stirred solution of 6-chloro-1,3-dimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidine-5-carbaldehyde (0.600 g, 2.96 mmol) and triethyl-amine (0.45 ml, 3.26 mmol) in dichloromethane (20 ml), a solution of N-phenylpiperazine (0.49 ml, 3.26 mmol) in dichloromethane (10 ml) was added dropwise. The resulting suspension was stirred at room temperature until the starting material was consumed (3.5 h, monitored by TLC). Then the reaction mixture was washed with water (3×10 ml), and the organic phase was dried over 20, anhydrous MgSO4. The solvent was evaporated in vacuo, and the brown oily crude product was purified by column chromatography with a mixture of dichloromethane:ethyl acetate (1:1) as the eluent and crystallized from ethanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536210B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-3688fac5655641648d7b461d2baad2b5 |
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| 出典メモ | uspto-grants-2013_09 |
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