Ethyl isocyanate → 5-Methoxy-3,6,7,8-tetrahydro-1,3-dimethylcyclopenta[d]pyrazolo[3,4-b]-pyridine

HRID 65019

Reaktionsgleichung

Reaktionsgleichung von HRID 65019
CN1[CH2:7][CH2:6][C:5]([C:8]2[C:9]([CH3:15])=[N:10][N:11]([CH3:14])[C:12]=2[NH2:13])=[CH:4][CH2:3]1.C(N=[C:19]=[O:20])C.N1C=CC(C)=C(C)[CH:22]=1>>[CH3:22][O:20][C:19]1[N:13]=[C:12]2[N:11]([CH3:14])[N:10]=[C:9]([CH3:15])[C:8]2=[C:5]2[CH2:6][CH2:7][CH2:3][C:4]=12

Komponenten

4

Edukt 3

HCID 8022Ethyl isocyanateHCID 114173,4-DimethylpyridineHCID 133521964-(1,2,5,6-tetrahydro-1-methyl-4-pyridinyl)-1,3-dimethyl 5-(1H)-pyrazolamine

Produkt 1

HCID 202349815-Methoxy-3,6,7,8-tetrahydro-1,3-dimethylcyclopenta[d]pyrazolo[3,4-b]-pyridine

Versuchsvorschrift

A mixture of 4-(1,2,5,6-tetrahydro-1-methyl-4-pyridinyl)-1,3-dimethyl-5-(1H)-pyrazolamine (2.06 g; 0.01 mol), 3,4-lutidine (20 ml), ethyl isocyanate (3.16 ml; 0.04 mol), under anhydrous conditions, are heated to the reflux temperature for about 3 hours. The mixture is then cooled to room temperature, concentrated under reduced pressure, washed with ethyl acetate and then with ethyl ether, thus obtaining the product of the title. M.p. 294°-297° C.

Aufarbeitung

  1. temperatureunder anhydrous conditions, are heated to the reflux temperature for about 3 hours
  2. concentrationconcentrated under reduced pressure
  3. washwashed with ethyl acetate
  4. customwith ethyl ether, thus obtaining the product of the title

Quellen und Nachweise

ORD-Eintrag
ord-253260bd1fa943b7ae013142de06fdeb
Quelldatensatz
uspto-grants-1986_09
Patentnummer
US04612318

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