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Triethylamine → 2-Methyl-5-[4-(2-nitro-phenyl)-piperazin-1-ylmethyl]-pyrimidin-4-ylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(2-Nitrophenyl)piperazine | HCID 100949 | — |
| 反応物 | 5-(Chloromethyl)-2-methylpyrimidin-4-amine--hydrogen chloride (1/1) | HCID 21473611 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Methyl-5-[4-(2-nitro-phenyl)-piperazin-1-ylmethyl]-pyrimidin-4-ylamine | HCID 21473662 | 76.1% |
反応手順
A solution of 1.25 g (0.0060 mol) of 1-(2-nitro-phenyl)-piperazine and 2.1 ml (0.015 mol) of triethylamine in 20 ml of dimethylformamide was treated with 0.97 g (0.0050 mol) of 5-chloromethyl-2-methyl-pyrimidin-4-ylamine hydrochloride and the mixture was stirred at room temperature under argon for 3 hours. The mixture was completely freed from the solvents and the residue was triturated in 20 ml of water. The resulting crystals were filtered off under suction, dried and chromatographed over silica gel with dichloromethane/methanol 19:1 as the eluent. 1.25 g (76%) of 2-methyl-5- [4-(2-nitro-phenyl )-piperazin-1-ylmethyl]-pyrimidin-4-ylamine were obtained as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05688798 |
| 出典データセット | uspto-grants-1997_11 |
| ORD ID | ord-fa14a891f71440eda38d04d4f8f6b9a3 |
| 出典メモ | uspto-grants-1997_11 |