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Triethylamine → 2-[4-(2-Furylcarbonyl)-1-piperazinyl]-4-methoxypyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(2-Furoyl)piperazine | HCID 550206 | — |
| 反応物 | 2-Chloro-4-methoxypyrimidine | HCID 588935 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | 2-[4-(2-Furylcarbonyl)-1-piperazinyl]-4-methoxypyrimidine | HCID 6919147 | 70.2% |
反応手順
A solution of 1.0 g (6.92 mmol) of 2-chloro-4-methoxypyrimidine, 1.49 g (8,30 mmol) of 1-(2-furylcarbonyl)piperazine and 1.39 g (13.84 mmol) of triethylamine in 20 mL of n-butanol is maintained under gentle reflux conditions overnight. The solvent is evaporated off under reduced pressure and the crude residue is diluted in chloroform and washed in water. The organic phase is dried over NaSO4 and evaporated to dryness to give a crude product which is purified using silica-gel chromatography eluting with ethyl acetate/petroleum ether 70:30 to yield an oil which solidifies when left to stand. The solid is suspended in petroleum ether to yield 1.4 g (4.86 mmol) of 2-[4-(2-furylcarbonyl)-1-piperazinyl]-4-methoxypyrimidine. m.p.=85-86° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06372746B1 |
| 出典データセット | uspto-grants-2002_04 |
| ORD ID | ord-823576c4dea949db9a3d27153e6f60b3 |
| 出典メモ | uspto-grants-2002_04 |