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3-Iodoaniline → N-(3-iodophenyl)-1,3-dimethyl-1H-pyrazole-5-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Iodoaniline | HCID 12271 | — |
| 反応物 | 2,5-Dimethyl-2H-pyrazole-3-carbonyl chloride | HCID 2736299 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | N-(3-iodophenyl)-1,3-dimethyl-1H-pyrazole-5-carboxamide | HCID 57657852 | — |
反応手順
To a solution of 3-iodoaniline (131 mg, 0.60 mmol) in 1.5 ml pyridine at room temperature was added over 2 minutes a solution of 1,3-dimethylpyrazole-5-carbonyl chloride (79 mg, 0.50 mmol) in 0.3 ml 1,2-dichloroethane. The reaction was stirred at room temperature for 30 minutes, quenched into a NaHCO3 solution, and extracted into EtOAc. The EtOAc solution was washed with NaHCO3 solution, brine, dried with anhydrous Na2SO4 and rotary evaporated. The resultant gummy solid was recrystallized from hexane/EtOAc to give the title compound as solid white needles (135 mg, 80%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08383825B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-4ef2056d8e3a4593a266deb313a0a3ac |
| 出典メモ | uspto-grants-2013_02 |