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Hydrochloric Acid → 3-Anilino-4-acetyl-5-methylpyrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Hydrazinecarbothioamide, N-phenyl- | HCID 730679 | — |
| 反応物 | 1-Chloro-2,4-pentanedione | HCID 14496856 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-Anilino-4-acetyl-5-methylpyrazole | HCID 20475377 | — |
反応手順
50 g of 4-phenylthiosemicarbazide is suspended in 300 ml of tetrahydrofuran and 0.5 ml of concentrated HCl is added. Then 40.4 g of 3-chloroacetyl acetone is allowed to run in all at once and the whole is cooled with an ice-bath. After 12 hours' stirring, the precipitate formed is suction filtered, washed with acetone and then boiled in a water/acetone mixture (1:1). This hot solution is filtered off from the sulfur and neutralized with aqueous ammonia solution. The product is then suction filtered and recrystallized from acetone; m.p. 246°-247° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04260775 |
| 出典データセット | uspto-grants-1981_04 |
| ORD ID | ord-6e8d420a9d6449bca3b577d317c15304 |
| 出典メモ | uspto-grants-1981_04 |