StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Dichloromethane → HCID 68756523, Verbindung

HRID 387558
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 387558
COC1C=CC(C[N:8]2[C:12]3=[N:13][CH:14]=[C:15]([C:30]4[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=4)[C:16]([N:17]4[CH2:22][CH2:21][N:20](C(OC(C)(C)C)=O)[CH2:19][CH2:18]4)=[C:11]3[CH:10]=[N:9]2)=CC=1.C(O)(C(F)(F)F)=O.C(Cl)[Cl:46]>>[ClH:46].[ClH:46].[C:30]1([C:15]2[C:16]([N:17]3[CH2:18][CH2:19][NH:20][CH2:21][CH2:22]3)=[C:11]3[CH:10]=[N:9][NH:8][C:12]3=[N:13][CH:14]=2)[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acid2×HCID 68764155tert-butyl 4-(1-(4-methoxybenzyl)-5-phenyl-1H-pyrazolo[3,4-b]pyridin-4-yl)piperazine-1-carboxylate

Produkt 1

HCID 68756523HCID 68756523, VerbindungAusbeute 75 %

Versuchsvorschrift

A solution of tert-butyl 4-(1-(4-methoxybenzyl)-5-phenyl-1H-pyrazolo[3,4-b]pyridin-4-yl)piperazine-1-carboxylate (0.440 g, 0.881 mmol) in DCM (5 mL) was added to TFA (1 mL) and stirred at room temperature for 1 hour. The reaction was then concentrated to dryness and dried under vacuum for 1 hour. TFA (3.39 mL, 44.0 mmol) was then added, and the mixture was stirred at 65° C. for 4 hours. The reaction was then concentrated to dryness, and the resulting residue was dissolved in DCM (3 mL). HCl in ether (2 mL, 2N) and ether (10 mL) were then added, and the resulting solid was collected by filtration to give 5-phenyl-4-(piperazin-1-yl)-1H-pyrazolo[3,4-b]pyridine dihydrochloride (0.29 g, 75%). MS ESI (+) m/z 280.1 detected.

Aufarbeitung

  1. concentrationThe reaction was then concentrated to dryness
  2. customdried under vacuum for 1 hour
  3. stirringthe mixture was stirred at 65° C. for 4 hours
  4. concentrationThe reaction was then concentrated to dryness
  5. dissolutionthe resulting residue was dissolved in DCM (3 mL)
  6. additionHCl in ether (2 mL, 2N) and ether (10 mL) were then added
  7. filtrationthe resulting solid was collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-89391c7063b742b6af71d771c25465b2
Quelldatensatz
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08372842B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion