関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | (1-Ethoxyethylidene)malononitrile | HCID 79450 | — |
| 反応物 | (2-Fluoro-4-methoxyphenyl)hydrazine | HCID 44203045 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5-amino-1-(2-fluoro-4-methoxyphenyl)-3-methyl-1H-pyrazole-4-carbonitrile | HCID 67120026 | 85% |
反応手順
To a stirred solution of 2-(1-ethoxyethylidene)malononitrile (167 mg, 1.23 mmol) was added (2-fluoro-4-methoxyphenyl)hydrazine (220 mg, 1.41 mmol) in EtOH (3 mL). The solution was heated to 105° C. in the microwave for 30 min. CH2Cl2 and 1 M HCl was added and separated, the organic extract was washed with aqueous NaHCO3. The solution was dried using a phase separator and concentrated under reduced pressure to give 5-amino-1-(2-fluoro-4-methoxyphenyl)-3-methyl-1H-pyrazole-4-carbonitrile (256 mg, 85%), which was used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08653112B2 |
|---|
| 出典データセット | uspto-grants-2014_02 |
|---|
| ORD ID | ord-2e7aadd7785c430dac02e54b8518cf76 |
|---|
| 出典メモ | uspto-grants-2014_02 |
|---|
