Diethyl Ether → 1-(Phenylcarbamoyl)-2-pyrazoline

HRID 274885

Reaktionsgleichung

Reaktionsgleichung von HRID 274885
[NH:1]1[CH2:5][CH2:4][CH:3]=[N:2]1.FC(F)(F)O[C:9]1[CH:14]=[CH:13][C:12]([N:15]=[C:16]=[O:17])=[CH:11][CH:10]=1.C(OCC)C>C(#N)C.C(N(CC)CC)C>[N:2]1([C:16]([NH:15][C:12]2[CH:13]=[CH:14][CH:9]=[CH:10][CH:11]=2)=[O:17])[CH2:3][CH2:4][CH:5]=[N:1]1

Komponenten

6

Edukt 3

HCID 3283Diethyl EtherHCID 669622-PyrazolineHCID 92298p-(Trifluoromethoxy)phenyl isocyanate

Produkt 1

HCID 226139461-(Phenylcarbamoyl)-2-pyrazoline

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8471TriethylamineKatalysatorHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

2.76 g (0,008 mol) of 3-(4'-chlorophenyl)-4-(4"-methyl-3"-trifluoromethyl-Δ2" -1",2",4"-triazolin-5"-on-1"-yl)-4,5-dihydropyrazole are dissolved in 20 ml of acetonitrile (anhydrous) at 60° C. until a clear solution has formed, this solution is treated with 1.7 g of 4-trifluoromethoxy-phenyl isocyanate, and 2drops of triethylamine are added. The mixture is subsequently allowed to stand for 2 hours at room temperature. The solvent is subsequently stripped off in vacuo, the residue is treated with 20 ml of diethyl ether and, after 2 hours, the precipitate which has formed is filtered off with suction. 2.0 g (45.6% of theory) of N-(4-trifluormethoxy)-3-(4'-chlorophenyl)-4-(4"-methyl-3"-trifluoromethyl-Δ2" -1",2",4,"-triazolin-5"-on-1"-yl)-4,5-dihydro-1-pyrazole-carboxanilide having a melting point of 241° C. are obtained.

Aufarbeitung

  1. customhas formed
  2. additionare added
  3. customthe precipitate which has formed
  4. filtrationis filtered off with suction

Quellen und Nachweise

ORD-Eintrag
ord-d1bc547f902d4e8f83b7be232363093c
Quelldatensatz
uspto-grants-1995_02
Patentnummer
US05391560

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