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Methylhydrazine → 1,3-dimethyl-4,5,6,7-tetrahydro-1H-indazol-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylhydrazine | HCID 6061 | — |
| 反応物 | 2-Acetyl-1,3-cyclohexanedione | HCID 138104 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1,3-dimethyl-4,5,6,7-tetrahydro-1H-indazol-4-one | HCID 14126679 | — |
反応手順
A solution of 11 ml of methylhydrazine in 50 ml of methanol was added dropwise to an ice-cold solution of 30 grams of 2-acetyl-1,3-cyclohexanedione in 200 ml of methanol and the reaction mixture was heated at reflux for 90 minutes. The solvent was removed under reduced pressure and the residue was triturated in hexane and cooled to give a clammy tan solid. This crude product was recrystallized from a mixture of toluene and hexane to give 1,5,6,7-tetrahydro-1,3-dimethyl-4H-indazol-4-one as a yellow crystalline solid melting at about 82.5°-84° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04734429 |
| 出典データセット | uspto-grants-1988_03 |
| ORD ID | ord-79223b7c48f14055a84d4da905beee2c |
| 出典メモ | uspto-grants-1988_03 |