Hydrochloric Acid → HCID 135554955, Verbindung

HRID 1379024Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1379024
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:16]([C:17]3[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=3)=[C:11]3[N:12]=[N:13][CH:14]=[CH:15][N:10]3[N:9]=2)=[CH:4][CH:3]=1.C([BH3-])#N.[Na+].Cl>CO>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:16]([C:17]3[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=3)=[C:11]3[NH:12][NH:13][CH2:14][CH2:15][N:10]3[N:9]=2)=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 5003444Sodium cyanoborohydrideHCID 22909019HCID 22909019, Verbindung

Produkt 1

HCID 135554955HCID 135554955, VerbindungAusbeute 92,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a suspension of 7-(4-fluorophenyl)-8-(pyridin-4-yl)pyrazolo[5,1-c][1,2,4]triazine (2.2 g) in methanol (20 ml) was added sodium cyanoborohydride (480 mg). The pH of the mixture was maintained at 3 to 4 for 2 hours with 1N hydrochloric acid. The procedure was repeated three additional times to completely finish the reduction. Then, the mixture was concentrated in vacuo and the residue was dissolved in 2N hydrochloric acid. The mixture was stirred at 80° C. for 30 minutes and cooled. The solution was neutralized with an aqueous saturated sodium bicarbonate solution. The separated solid was collected, washed with water and methanol and dried to give 7-(4-fluorophenyl)-8-(pyridin-4-yl)-1,2,3,4-tetrahydropyrazolo[5,1-c][1,2,4]triazine (2.06 g).

Aufarbeitung

  1. concentrationThen, the mixture was concentrated in vacuo
  2. dissolutionthe residue was dissolved in 2N hydrochloric acid
  3. temperaturecooled
  4. customThe separated solid was collected
  5. washwashed with water and methanol
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-f2d638b3eeef4d48b17ef22c64f2366c
Quelldatensatz
uspto-grants-1997_09
Patentnummer
US05670503

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