Hydrochloric Acid → HCID 20509910, Verbindung

HRID 1758235Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1758235
COC(OC)CNCC1C=C(C)C=CC=1N.N#CBr.[NH2:20][C:21]1[N:30]([CH2:31][CH:32](OC)OC)[CH2:29][C:28]2[C:23](=[CH:24][CH:25]=[C:26]([CH3:37])[CH:27]=2)[N:22]=1.Cl>C(O)C>[CH3:37][C:26]1[CH:27]=[C:28]2[C:23](=[CH:24][CH:25]=1)[NH:22][C:21]1=[N:20][CH:32]=[CH:31][N:30]1[CH2:29]2

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 10476Cyanogen BromideHCID 20509899HCID 20509899, VerbindungHCID 20509920HCID 20509920, Verbindung

Produkt 1

HCID 20509910HCID 20509910, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

45 g of N-(2-amino-5-methylbenzyl)-aminoacetaldehydedimethylacetal obtained in step (d) and 25 g of cyanogen bromide are heated under reflux in 500 ml of 95% ethanol for 18 hours. After the mixture containing 2-amino-3-(2,2-dimethoxyethyl)-6-methyl-3,4-dihydroquinazoline is cooled, 200 ml of 5 N hydrochloric acid are added, and the solution is left to stand for 2 hours at room temperature. After the reaction solution is concentrated in a vacuum, it is made alkaline with dilute caustic soda, whereupon the title compound crystallizes out, and is recrystallised from methanol or ethanol. M.p. 265° C.

Aufarbeitung

  1. temperatureis cooled
  2. waitthe solution is left
  3. concentrationAfter the reaction solution is concentrated in a vacuum, it
  4. customwhereupon the title compound crystallizes out, and
  5. customis recrystallised from methanol or ethanol

Quellen und Nachweise

ORD-Eintrag
ord-cff7473dd8184b4fa574fa6adafe38ac
Quelldatensatz
uspto-grants-1983_02
Patentnummer
US04372956

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