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

HRID 1410140노트

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HRID 1410140 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
105 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-8a99dcf7096b4a93ac32f0df757a3d88
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08921402B2

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