Pyridinium chloride → HCID 68554841, Verbindung

HRID 2359883Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2359883
C[O:2][C:3]1[CH:20]=[CH:19][CH:18]=[CH:17][C:4]=1[CH2:5][N:6]1[CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:8]=[C:7]1[NH2:16].Cl.N1C=CC=CC=1>O>[NH2:16][C:7]1[N:6]([CH2:5][C:4]2[CH:17]=[CH:18][CH:19]=[CH:20][C:3]=2[OH:2])[CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:8]=1

Komponenten

4

Edukt 2

HCID 10176127Pyridinium chlorideHCID 68550921HCID 68550921, Verbindung

Produkt 1

HCID 68554841HCID 68554841, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

120 mg (0.45 mmol) 3-(2-methoxybenzyl)-3,4-dihydroquinazolin-2-amine and 5 g pyridine hydrochloride were combined and heated for 4 hours at approx. 140° C. After cooling the melt, the residue was dissolved in water, extracted three times with dichloromethane and the combined organic phases were dried, filtered and evaporated. The resulting crude product was purified over MPLC (silica gel: Bischoff Prontoprep 60-2540-C18E, 32 μm; mobile phase: CH3CN/H2O+0.1% acetic acid) and subsequent lyophilization yielded the target product as a beige white solid; 110 mg.

Aufarbeitung

  1. temperatureAfter cooling the melt
  2. extractionextracted three times with dichloromethane
  3. customthe combined organic phases were dried
  4. filtrationfiltered
  5. customevaporated
  6. customThe resulting crude product was purified over MPLC (silica gel: Bischoff Prontoprep 60-2540-C18E, 32 μm; mobile phase: CH3CN/H2O+0.1% acetic acid) and subsequent lyophilization

Quellen und Nachweise

ORD-Eintrag
ord-e27a5b14b6bc467db73f5f03f6a8c3b8
Quelldatensatz
uspto-grants-2014_04
Patentnummer
US08686002B2

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