Potassium bisulfate → 1,1-Bis(2,4-dimethylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethene

HRID 974473

Reaktionsgleichung

Reaktionsgleichung von HRID 974473
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[C:9]([C:18]1[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][C:19]=1[CH3:25])(O)[CH2:10][C:11]1[N:15]([CH3:16])[N:14]=[N:13][N:12]=1.S([O-])(O)(=O)=O.[K+]>C(Cl)Cl>[CH3:25][C:19]1[CH:20]=[C:21]([CH3:24])[CH:22]=[CH:23][C:18]=1[C:9]([C:3]1[CH:4]=[CH:5][C:6]([CH3:8])=[CH:7][C:2]=1[CH3:1])=[CH:10][C:11]1[N:15]([CH3:16])[N:14]=[N:13][N:12]=1

Komponenten

4

Edukt 2

HCID 516920Potassium bisulfateHCID 147239461,1-Bis(2,4-dimethylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanol

Produkt 1

HCID 147239471,1-Bis(2,4-dimethylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)etheneAusbeute 69,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 1,1-bis(2,4-dimethylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanol (1.8 g, 5.4 mmoles) and potassium hydrogen sulfate (100 mg) was placed in an oil bath preheated to 190° C. After 15 minutes, the melt was cooled and methylene chloride added to the residue. The insolubles were removed and the solution evaporated. The residue was crystallized from isopropyl ether to give 1.2 g of the title compound; m.p.=143°-143.5° C.

Aufarbeitung

  1. customwas placed in an oil bath
  2. custompreheated to 190° C
  3. temperaturethe melt was cooled
  4. customThe insolubles were removed
  5. customthe solution evaporated
  6. customThe residue was crystallized from isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-334f0c84d6c9461490ba524d64b0f3aa
Quelldatensatz
uspto-grants-1991_11
Patentnummer
US05068346

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