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Hydrochloric Acid → 1-(2-Furoyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Furancarbonyl chloride | HCID 68242 | — |
| 反応物 | Piperazine, hexahydrate | HCID 120181 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(2-Furoyl)piperazine | HCID 550206 | 60% |
反応手順
This compound and its preparation has been described in Great Britain Patents 1,390,014 and 1,390,015. Piperazine hexahydrate (194 g, 1 mole) was dissolved in 250 ml H2O. The solution was acidified to pH 4.5 with 6N HCl. Furoyl chloride (130.5 g, 1 mole, Aldrich) was added along with 10% NaOH solution at such a rate that the pH was maintained at 4.5. After 1 hour, the solution was made basic (pH=8.5) with NaOH solution. The reaction mixture was continuously extracted with chloroform for 36 hours. The CHCl3 extract was dried over MgSO4, and filtered. Distillation gave 108.2 g product (60%), b.p. 132°-138° C./0.6 mm Hg, m.p. 69°-70° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05861309 |
| 出典データセット | uspto-grants-1999_01 |
| ORD ID | ord-82c6f48e8cf44601ac4c07201fdf6858 |
| 出典メモ | uspto-grants-1999_01 |