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Cyclohexanol → 6-(2-Chlorophenyl)-7-(4-chlorophenyl)-3-(cyclohexyloxy)-[1,2,4]triazolo[4,3-b]pyridazine

HRID 1867873
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1867873
[CH:1]1([OH:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Na].Cl[C:10]1[N:14]2[N:15]=[C:16]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=3[Cl:32])[C:17]([C:19]3[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=3)=[CH:18][C:13]2=[N:12][N:11]=1>C1COCC1>[Cl:32][C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][C:26]=1[C:16]1[C:17]([C:19]2[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=2)=[CH:18][C:13]2[N:14]([C:10]([O:7][CH:1]3[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]3)=[N:11][N:12]=2)[N:15]=1
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Komponenten

5

Edukt 3

HCID 7966CyclohexanolHCID 5360545SodiumHCID 579797573-Chloro-6-(2-chlorophenyl)-7-(4-chlorophenyl)-[1,2,4]triazolo[4,3-b]pyridazine

Produkt 1

HCID 119930186-(2-Chlorophenyl)-7-(4-chlorophenyl)-3-(cyclohexyloxy)-[1,2,4]triazolo[4,3-b]pyridazineAusbeute 7,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028
Tetrahydrofuran
Lösungsmittel

Versuchsvorschrift

To a solution of cyclohexanol (0.5 g, 5 mmol) in anhydrous THF (1 mL) at room temperature was added freshly cut sodium metal (35 mg, 1.5 mmol). The reaction mixture was stirred at room temperature for 20 min, then at 60° C. for 30 min, and then allowed to cool to room temperature. Into this mixture was added 3-chloro-6-(2-chlorophenyl)-7-(4-chlorophenyl)-[1,2,4]triazolo[4,3-b]pyridazine (115 mg, 0.3 mmol), the resulting mixture was stirred at room temperature under argon for 16 h. The reaction was carefully quenched by addition of methanol, then diluted with EtOAc. The solution was washed with H2O, saturated aqueous NaCl, dried (Na2SO4), filtered and concentrated. The obtained residue was purified using a silica gel cartridge (12 g) eluting with a gradient of EtOAc (0-40%) in hexanes to afford 10 mg (7.6%) of the title compound as a pale-yellow solid. HPLC/MS (method A): retention time=4.06 min, (M+H)+=439.1. 1H NMR (CDCl3, 400 MHz): δ 7.84 (s, 1H), 7.46 (dd, J=5.62, 3.67 Hz, 1H), 7.32-7.37 (m, 2H), 7.25-7.30 (m, 1H), 7.20 (d, J=8.56 Hz, 2H), 7.03-7.08 (m, 2H), 5.21-5.29 (m, 1H), 2.28 (d, J=12.96 Hz, 2H), 1.88 (d, J=4.40 Hz, 2H), 1.60-1.80 (m, 3H), 1.45-1.52 (m, 2H), 1.20-1.40(m, 1H).

Aufarbeitung

  1. waitat 60° C. for 30 min
  2. temperatureto cool to room temperature
  3. stirringthe resulting mixture was stirred at room temperature under argon for 16 h
  4. customThe reaction was carefully quenched by addition of methanol
  5. additiondiluted with EtOAc
  6. washThe solution was washed with H2O, saturated aqueous NaCl
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customThe obtained residue was purified
  11. washeluting with a gradient of EtOAc (0-40%) in hexanes

Quellen und Nachweise

ORD-Eintrag
ord-430638d8d44b4a0086789165a1a62754
Quelldatensatz
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07632837B2

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