Water → alpha,alpha-Bis(4-chlorophenyl)-1H-pyrazole-4-methanol

HRID 64634ノート

反応式

HRID 64634 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=2)([C:10]2[CH:11]=[N:12]C=[N:14][CH:15]=2)[OH:9])=[CH:4][CH:3]=1.NN.O>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=2)([C:10]2[CH:11]=[N:12][NH:14][CH:15]=2)[OH:9])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 962WaterHCID 9321HydrazineHCID 161536LY 43578

生成物 1

HCID 13672688alpha,alpha-Bis(4-chlorophenyl)-1H-pyrazole-4-methanol

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The methiodide salt of α,α-bis(4-chlorophenyl)-pyrimidine-5-methanol (12.8 g) was heated to reflux with 3 g of anhydrous hydrazine in ethanol. The original slurry went into solution and then a precipitate formed, at which time 25 ml of water were added. The mixture was heated at reflux for 20 minutes, filtered hot, water was added and the mixture was extracted with ether. The ether was evaporated and the residue was crystallized from chloroform to provide the title product, m.p. 135°-137° C. The NMR and mass spectra were consistent with the desired structure.

後処理

  1. additionwere added
  2. temperatureThe mixture was heated
  3. temperatureat reflux for 20 minutes
  4. filtrationfiltered hot
  5. additionwater was added
  6. extractionthe mixture was extracted with ether
  7. customThe ether was evaporated
  8. customthe residue was crystallized from chloroform

出典と根拠

ORDレコード
ord-883462650c1c42c3bb7da08a9468e273
出典データセット
uspto-grants-1986_09
特許番号
US04609666

反応ノート

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