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Heptane → 5-Methyl-3-phenyl-4-isoxazolecarbohydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Heptane | HCID 8900 | — |
| 反応物 | 5-Methyl-3-phenylisoxazole-4-carboxylic acid | HCID 14343 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-Methyl-3-phenyl-4-isoxazolecarbohydrazide | HCID 727924 | 85% |
反応手順
To a solution of 5-methyl-3-phenyl-isoxazole-4-carboxylic acid (5.00 g, 24.6 mmol) in THF (50 mL) was added in one portion 1,1′-carbonyl-diimidazole (4.39 g, 27.1 mmol). After stirring for 15 min at ambient temperature the solution was warmed to 70° C. and stirred for 30 min at this temperature. After the solution was cooled to 0° C. hydrazine monohydrate (2.4 mL, 49.0 mmol) was added over a period of 2 min while the temperature raised to 15° C. The resulting suspension was stirred for 30 min at 0° C. After addition of 20 mL heptane the suspension was stirred for 15 min at 0° C. and filtered off. Washing with water and drying afforded the title compound (4.52 g, 85%) as a white solid. MS: m/e=218.2 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07541372B2 |
| 出典データセット | uspto-grants-2009_06 |
| ORD ID | ord-b6859324313a427eba4754a44a3585f4 |
| 出典メモ | uspto-grants-2009_06 |