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Methylhydrazine → 4-(Aminomethyl)-3-cyclopropyl-1,2,4-oxadiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylhydrazine | HCID 6061 | — |
| 反応物 | N-[(3-cyclopropyl-1,2,4-oxadiazol-5-yl)methyl]phthalimide | HCID 22713498 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 4-(Aminomethyl)-3-cyclopropyl-1,2,4-oxadiazole | HCID 22713490 | — |
反応手順
N-[(3-Cyclopropyl-1,2,4-oxadiazol-5-yl)methyl]phthalimide (104 g, 387 mmol) was dissolved in 1,2-dichloroethane (500 mL), N-methylhydrazine (22.4 mL, 426 mmol) was added and the solution was refluxed for 5 h. The suspension was cooled in ice, the precipitate (2-methyl-2,3-dihydro-phthalazine-1,4-dione) was filtered off and washed with 1,2-dichloroethane (100 mL). The filtrate was evaporated and the residue distilled at 70° C./0.4 mbar (bath-T 100-150° C). Yield: 39.3 g (73%). m/z 139 (M).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06743789B2 |
| 出典データセット | uspto-grants-2004_06 |
| ORD ID | ord-690efa1200264a80a13c5dfe52644e48 |
| 出典メモ | uspto-grants-2004_06 |