Hydrochloric Acid → HCID 385229, Verbindung

HRID 1421878Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1421878
[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2([CH2:18][OH:19])[CH2:13][C:12](OC)([O:14]C)[CH2:11]2)[CH:5]=[C:4]([Cl:20])[N:3]=1.Cl.N.CO>CC(C)=O>[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2([CH2:18][OH:19])[CH2:11][C:12](=[O:14])[CH2:13]2)[CH:5]=[C:4]([Cl:20])[N:3]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 385228HCID 385228, VerbindungHCID 21705897Ammonia methanol

Produkt 1

HCID 385229HCID 385229, VerbindungAusbeute 70,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

To 2-amino-6-chloro-4-[[(1-hydroxymethyl-3,3-dimethoxy-1-cyclobutyl)methyl]amino]pyrimidine (0.61 g, 2.0 mmol) were added acetone (50 ml) and 20% hydrochloric acid (0.5 ml), and the mixture was refluxed for 30 minutes. The mixture was neutralized with 10% ammonia-methanol under ice-cooling. The solvent was distilled away under reduced pressure and the residue was recrystallized from acetone to give colorless prism crystals (0.36 g, 70.1%), m.p. 171-173° C. (acetone).

Aufarbeitung

  1. temperaturethe mixture was refluxed for 30 minutes
  2. temperaturecooling
  3. distillationThe solvent was distilled away under reduced pressure
  4. customthe residue was recrystallized from acetone

Quellen und Nachweise

ORD-Eintrag
ord-50cc90d356d346138ecfc11fd296e9f7
Quelldatensatz
uspto-grants-2000_06
Patentnummer
US06080750

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