p-Toluenesulfonic acid → 1,1-Bis(2-fluoro-4-methylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethene

HRID 330677

Reaktionsgleichung

Reaktionsgleichung von HRID 330677
[F: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[F:25])(O)[CH2:10][C:11]1[N:15]([CH3:16])[N:14]=[N:13][N:12]=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1.C(OCC)C>[F: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[F:1])=[CH:10][C:11]1[N:15]([CH3:16])[N:14]=[N:13][N:12]=1

Komponenten

5

Edukt 2

HCID 6101p-Toluenesulfonic acidHCID 147239921,1-Bis(2-fluoro-4-methylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanol

Produkt 1

HCID 147239931,1-Bis(2-fluoro-4-methylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethene

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

A suspension of 1,1-bis(2-fluoro-4-methylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanol (7.3 g, 21.0 mmoles) in toluene (200 mL) with p-toluene sulfonic acid (3 g) and the mixture heated at reflux for 14 hours. After cooling, the mixture was diluted with diethyl ether and extracted with saturated sodium bicarbonate solution and water. The organic layer was dried (MgSO4) and evaporated. The residue was triturated with isopropyl ether to give the title compound; m.p.=58°-60° C.

Aufarbeitung

  1. temperaturethe mixture heated
  2. temperatureat reflux for 14 hours
  3. temperatureAfter cooling
  4. extractionextracted with saturated sodium bicarbonate solution and water
  5. dry with materialThe organic layer was dried (MgSO4)
  6. customevaporated
  7. customThe residue was triturated with isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-a74c99d3c3514bdbb13a65d5dad474f5
Quelldatensatz
uspto-grants-1990_01
Patentnummer
US04897490

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