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Potassium Carbonate → Pyrimidine, 2-(4-(1,4-benzodioxin-6-ylmethyl)-1-piperazinyl)-, dihydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Chloropyrimidine | HCID 74404 | — |
| 反応物 | 1-(6-Benzodioxinyl methyl)piperazine | HCID 70455395 | — |
| 溶媒 | 1-Pentanol | HCID 6276 | — |
| 生成物 | Pyrimidine, 2-(4-(1,4-benzodioxin-6-ylmethyl)-1-piperazinyl)-, dihydrochloride | HCID 3071330 | 156.5% |
反応手順
A solution of 11.4 g (0.1 mole) of 2-chloropyrimidine and 23.2 g (0.1 mole) of 1-(6-benzodioxinyl methyl)piperazine (oil) in 500 ml of pentanol, as refluxed for 6 hours, in the presence of 13.8 g (0.1 mole) of potassium carbonate. After the completion of the reaction, the so-formed salt was filtered off and the solvent was evaporated under reduced pressure. The so-obtained oily residue (30 g) was dissolved in 160 ml of anhydrous ethanol. After addition of an excess of hydrochloric acid ether solution, the dihydrochloride crystallises. 30 g of 1-(benzodioxin-6-yl methyl)-4-(pyrimidin-2-yl)piperazine dihydrochloride white crystals were finally obtained, melting at 215°-220° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04613601 |
| 出典データセット | uspto-grants-1986_09 |
| ORD ID | ord-446e8a80fd7642449b2d5bff95ba4b59 |
| 出典メモ | uspto-grants-1986_09 |