Potassium Carbonate → HCID 57425811, Verbindung

HRID 1363641Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1363641
[CH3:1][C:2]1[S:6][C:5]([CH2:7]CS([O-])(=O)=O)=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14].FC(F)(F)C1N=C(C(F)(F)F)NN=1.C(=O)([O-])[O-:30].[K+].[K+].C1OCCOCCOCCOCCOCCOC1>C(#N)C>[CH3:1][C:2]1[S:6][C:5]([CH2:7][OH:30])=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14]

Komponenten

6

Edukt 4

HCID 11430Potassium CarbonateHCID 2855718-Crown-6HCID 146885163,5-Bis(trifluoromethyl)-1H-1,2,4-triazoleHCID 86626337HCID 86626337, Verbindung

Produkt 1

HCID 57425811HCID 57425811, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

1.0 g (3.98 mmol) (5-methyl-4-nitro-2-thienyl)methylmethane sulphonate, 0.82 g (3.98 mmol) 3,5-bis(trifluoromethyl)-1H-1,2,4-triazole, 0.93 g (5.97 mmol) potassium carbonate and 0.11 g (0.398 mmol) 18-crown-6 are heated under reflux in acetonitrile for 2 h. The cooled reaction mixture is evaporated, the residue taken up in 20 ml water and extracted three times with ethyl acetate. The combined organic phases are washed with saturated sodium chloride solution, dried over sodium sulphate and the solvent is distilled off under vacuum. The product (1-[(5-methyl-4-nitro-2-thienyl)methyl]-3,5-bis(trifluoromethyl)-1H-1,2,4-triazole) is used in the next stage without purification.

Aufarbeitung

  1. customThe cooled reaction mixture
  2. customis evaporated
  3. extractionextracted three times with ethyl acetate
  4. washThe combined organic phases are washed with saturated sodium chloride solution
  5. dry with materialdried over sodium sulphate
  6. distillationthe solvent is distilled off under vacuum
  7. customThe product (1-[(5-methyl-4-nitro-2-thienyl)methyl]-3,5-bis(trifluoromethyl)-1H-1,2,4-triazole) is used in the next stage without purification

Quellen und Nachweise

ORD-Eintrag
ord-cfca1f7d771c48d9bd45b50a59b49e03
Quelldatensatz
uspto-grants-2011_02
Patentnummer
US07884242B2

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