Hydrochloric Acid → 1-(4-Chlorophenyl)-1H-pyrazol-5-amine

HRID 459672노트

반응식

HRID 459672 반응식
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][NH2:10])=[CH:5][CH:4]=1.Cl.CN([C:15](=[CH2:18])[C:16]#[N:17])C>CO>[NH2:17][C:16]1[N:9]([C:6]2[CH:7]=[CH:8][C:3]([Cl:2])=[CH:4][CH:5]=2)[N:10]=[CH:18][CH:15]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 71600Hydrazine, (4-chlorophenyl)-, hydrochloride (1:1)HCID 12896101Dimethylaminoacrylonitrile

생성물 1

HCID 122043801-(4-Chlorophenyl)-1H-pyrazol-5-amine

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

21.5 g (0.12 mol) of 4-chlorophenylhydrazine hydrochloride was suspended in 150 mL of methanol, 5 mL of concentrated hydrochloric acid was added, and the mixture was heated at reflux, which gave a clear, yellow-brown solution. To this solution was added dropwise 11.5 g (0.12 mol) of dimethylaminoacrylonitrile over a period of 30 minutes. After 1.5 h at reflux, most of the solvent was removed under vacuum. The remaining residue was taken up in 40 mL of dimethylformamide, and 9 mL of concentrated ammonia solution was added at room temperature. The resulting white precipitate was filtered off and discarded. The clear filtrate was used in Step 10.2 without further purification.

후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux
  3. customwhich gave a clear, yellow-brown solution
  4. temperatureAfter 1.5 h at reflux, most of the solvent
  5. customwas removed under vacuum
  6. addition9 mL of concentrated ammonia solution was added at room temperature
  7. filtrationThe resulting white precipitate was filtered off
  8. customThe clear filtrate was used in Step 10.2 without further purification

출처 및 근거

ORD 기록
ord-bce34b5d0e8f40b482936010394f4599
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07195649B2

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