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1-(3-Chlorophenyl)piperazine → 5-[4-(3-Chloro-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(3-Chlorophenyl)piperazine | HCID 1355 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-(Bromomethyl)pyrimidine-2,4-diamine dihydrobromide | HCID 21473608 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-[4-(3-Chloro-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine | HCID 21473673 | 63% |
反応手順
A solution of 13.5 g (0.050 mol) of 1-(3-chloro-phenyl)-piperazine in 500 ml of tetrahydrofuran was treated with 35 ml (0.25 mol) of triethylamine and 18.2 g (0.050 mol) of 5-bromomethyl-pyrimidine-2,4-diamine dihydrobromide and the mixture was stirred at room temperature under argon for 16 hours. The suspension obtained was suction filtered and the filtrate was completely freed from the solvents. The residue was chromatographed over silica gel with acetonitrile/methanol 1:1 as the eluent and digested in diethyl ether. 10 g (63%) of 5-[4-(3-chloro-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine were obtained as beige crystals; m.p. 222°-226°.
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-82a69ec5510545d78b21805f22dd62c6 |
| 出典メモ | uspto-grants-1997_11 |