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

HRID 459672ノート

反応式

HRID 459672 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bce34b5d0e8f40b482936010394f4599
出典データセット
uspto-grants-2007_03
特許番号
US07195649B2

反応ノート

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