Formaldehyde → 1-(4-Chlorophenylthio)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pentan-3-one

HRID 255812

반응식

HRID 255812 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[CH:4][CH:3]=1.[CH3:9][C:10]([C:13]([CH2:15][N:16]1[N:20]=[CH:19][N:18]=[CH:17]1)=[O:14])([CH3:12])[CH3:11].C=O.N1CCCC[CH2:24]1>C1(C)C=CC=CC=1.O.C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:24][CH:15]([N:16]2[CH:17]=[N:18][CH:19]=[N:20]2)[C:13](=[O:14])[C:10]([CH3:9])([CH3:11])[CH3:12])=[CH:4][CH:3]=1

참가 물질

8

반응물 4

HCID 712FormaldehydeHCID 7815p-ChlorothiophenolHCID 8082PiperidineHCID 1008773,3-Dimethyl-1-(1H-1,2,4-triazol-1-yl)-2-butanone

생성물 1

HCID 131913651-(4-Chlorophenylthio)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pentan-3-one수율 28%

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 962Water용매HCID 1140Toluene용매

실험 절차

A mixture of 72.5 g (0.5 mol) of 4-chlorothiophenol, 100.2 g (0.6 mol) of 1,2,4-triazol-1-yl-pinacolin, 18 g (0.6 mol) of paraformaldehyde, 15 g of acetic acid and 5 ml of piperidine in 600 ml of toluene was heated under reflux in a water separator. After the water has been separated off, the reaction solution was washed with water, dried over sodium sulphate, filtered, and concentrated in vacuo. The oily residue was chromatographed over a silica gel column (mobile phase: chloroform). 45 g (28% of theory) of 1-(4-chlorophenylthio)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pentan -3-one of melting point 67° C. were obtained.

후처리

  1. temperaturewas heated
  2. customAfter the water has been separated off
  3. washthe reaction solution was washed with water
  4. dry with materialdried over sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe oily residue was chromatographed over a silica gel column (mobile phase: chloroform)

출처 및 근거

ORD 기록
ord-928c673c32af4ee084ea5f08ee68500e
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04699645

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