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Triethylamine → 5-(4-p-Tolyl-piperazin-1-ylmethyl)-pyrimidine-2,4-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(p-Tolyl)piperazine | HCID 83113 | — |
| 反応物 | 5-(Bromomethyl)pyrimidine-2,4-diamine dihydrobromide | HCID 21473608 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-(4-p-Tolyl-piperazin-1-ylmethyl)-pyrimidine-2,4-diamine | HCID 21473633 | 51.1% |
反応手順
A solution of 0.87 g (0.00493 mol) of 1-p-tolyl-piperazine in 30 ml of dimethylformamide was treated with 1.37 ml (0.00986 mol) of triethylamine and 0.60 g (0.00164 mol) of 5-bromomethyl-pyrimidine-2,4-diamine dihydrobromide and the mixture was stirred at room temperature under argon for 110 hours. The mixture was completely freed from the solvents. The residue was chromatographed over silica gel with methanol as the eluent, digested in dichloromethane/water 1:1 and subsequently filtered off under suction. 0.25 g (51%) of 5-(4-p-tolyl-piperazin-1-ylmethyl)-pyrimidine-2,4-diamine was obtained as beige crystals; m.p. 248°-250°.
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-521d9de644634cf084fe6b6c555047c4 |
| 出典メモ | uspto-grants-1997_11 |