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Potassium Carbonate → HCID 13374747、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-(3-Chlorophenyl)piperazine monohydrochloride | HCID 25681 | — |
| 反応物 | 1-Bromo-4-chlorobutane | HCID 81364 | — |
| 反応物 | Sodium 1,2,4-Triazolo[4,3-a]pyridin-3(2H)-one | HCID 70507128 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | HCID 13374747 | HCID 13374747 | 43% |
反応手順
A mixture of 8.0 g. (0.0343 mole) of 1-(3-chlorophenyl)piperazine hydrocloride, 5.88 g. (0.0343 mole) of 1-bromo-4-chlorobutane, 9.48 g. (0.9686 mole) of finely powdered potassium carbonate, and 200 ml. of dry xylene was refluxed for 22 hr. To this mixture there was then added 5.39 g. (0.0343 mole) of sodium 1,2,4-triazolo[4,3-a]pyridin-3(2H)-one, and the resulting suspension was refluxed an additional 72 hr. The mixture was then cooled, diluted with 200 ml. of chloroform, stirred for 15 min. and filtered. The clear filtrate was concentrated to an oil (9.8 g.) under reduced pressure. The residue was recrystallized from ET2O--EtOH--CHCl3 to afford 2.31 g. (43%) of the desired product, m.p. 122°-123°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04465683 |
| 出典データセット | uspto-grants-1984_08 |
| ORD ID | ord-9921cd8d05fa42deba4b5fc11d0e9396 |
| 出典メモ | uspto-grants-1984_08 |