Water → HCID 839770, Verbindung

HRID 1076355Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1076355
Cl[C:2]1[N:11]=[C:10](Cl)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[NH:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1.O>O1CCCC1>[N:13]1([C:2]2[N:11]=[C:10]([N:13]3[CH2:17][CH2:16][CH2:15][CH2:14]3)[C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[N:3]=2)[CH2:17][CH2:16][CH2:15][CH2:14]1

Komponenten

5

Edukt 3

HCID 962WaterHCID 31268PyrrolidineHCID 2528862,4-Dichloroquinazoline

Produkt 1

HCID 839770HCID 839770, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Ten grams of 2,4-dichloroquinazoline was added carefully to a solution of 25 ml of pyrrolidine in 200 ml of tetrahydrofuran. The resulting mixture was heated at reflux overnight and then was poured into a mixture of ice and water. The resulting mixture was extracted several times with ether. The ether extracts were combined and washed with water. The ether phase then was dried over anhydrous sodium sulfate. The solvent was removed by distillation and the residue was recrystallized from a 1:1 benzene:hexane mixture to give 10.1 g of 2,4-bispyrrolidinylquinazoline; m.p. 127°-129°. The following analytical data were obtained:

Aufarbeitung

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux overnight
  3. extractionThe resulting mixture was extracted several times with ether
  4. washwashed with water
  5. dry with materialThe ether phase then was dried over anhydrous sodium sulfate
  6. customThe solvent was removed by distillation
  7. customthe residue was recrystallized from a 1:1 benzene

Quellen und Nachweise

ORD-Eintrag
ord-a5401a0c98174433a795e85e88baa321
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03956495

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