Hydrochloric Acid → 5-amino-1-(2-fluoro-4-methoxyphenyl)-3-methyl-1H-pyrazole-4-carbonitrile

HRID 1410140ノート

反応式

HRID 1410140 の反応式
C(O[C:4](=[C:6]([C:9]#[N:10])[C:7]#[N:8])[CH3:5])C.[F:11][C:12]1[CH:17]=[C:16]([O:18][CH3:19])[CH:15]=[CH:14][C:13]=1[NH:20][NH2:21].C(Cl)Cl.Cl>CCO>[NH2:10][C:9]1[N:20]([C:13]2[CH:14]=[CH:15][C:16]([O:18][CH3:19])=[CH:17][C:12]=2[F:11])[N:21]=[C:4]([CH3:5])[C:6]=1[C:7]#[N:8]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 79450(1-Ethoxyethylidene)malononitrileHCID 44203045(2-Fluoro-4-methoxyphenyl)hydrazine

生成物 1

HCID 671200265-amino-1-(2-fluoro-4-methoxyphenyl)-3-methyl-1H-pyrazole-4-carbonitrile収率 85%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
105 °C

実験手順

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.

後処理

  1. customseparated
  2. extractionthe organic extract
  3. washwas washed with aqueous NaHCO3
  4. customThe solution was dried
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-8a99dcf7096b4a93ac32f0df757a3d88
出典データセット
uspto-grants-2014_12
特許番号
US08921402B2

反応ノート

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