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1,1'-Carbonyldiimidazole → 5-chloro-1-methyl-N-cyclopropyl-1H-pyrazole-4-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 反応物 | Cyclopropylamine | HCID 69828 | — |
| 反応物 | 5-Chloro-1-methyl-1H-pyrazole-4-carboxylic acid | HCID 2735774 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-chloro-1-methyl-N-cyclopropyl-1H-pyrazole-4-carboxamide | HCID 13821989 | 116.9% |
反応手順
Carbonyldiimidazole (3.6 grams, 0.022 mole) was added to a solution of 5-chloro-1-methyl-1H-pyrazole-4-carboxylic acid (2.4 grams, 0.015 mole) in 40 ml. of tetrahydrofuran, and the solution was stirred at room temperature for twenty minutes. Cyclopropylamine (1.3 grams, 0.022 mole) was then added and the reaction mixture was stirred at room temperature for sixteen hours. Solvent was removed in vacuo and the residue was taken up in 250 ml. of chloroform, washed with water, washed with saturated brine, and dried using sodium sulfate and filter paper. The product was recrystallized from toluene, yielding 3.5 grams of 5-chloro-1-methyl-N-cyclopropyl-1H-pyrazole-4-carboxamide, mp=105°-107° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04620865 |
| 出典データセット | uspto-grants-1986_11 |
| ORD ID | ord-d38bd1c3d665459f8a8ea4d2f94daa22 |
| 出典メモ | uspto-grants-1986_11 |