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

HRID 64634노트

반응식

HRID 64634 반응식
[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

참가 물질

5

반응물 3

HCID 962WaterHCID 9321HydrazineHCID 161536LY 43578

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-883462650c1c42c3bb7da08a9468e273
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04609666

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