Ammonia → HCID 385198, Verbindung

HRID 1421876Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1421876
[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2([CH2:14][OH:15])[CH2:13][CH2:12][CH2:11]2)[CH:5]=[CH:4][N:3]=1.C([O-])(=O)C.[Na+].[Br:21]Br.N>C(O)(=O)C.O>[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2([CH2:14][OH:15])[CH2:13][CH2:12][CH2:11]2)[C:5]([Br:21])=[CH:4][N:3]=1

Komponenten

7

Edukt 4

HCID 222AmmoniaHCID 24408BromineHCID 385194HCID 385194, VerbindungHCID 517045Sodium Acetate

Produkt 1

HCID 385198HCID 385198, VerbindungAusbeute 72,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittel2×HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

To 2-amino-4-[[(1-hydroxymethyl-1-cyclobutyl)methyl]amino]pyrimidine (0.21 g, 1.0 mmol) was added acetic acid (3 ml) and the mixture was heated to 110° C. Sodium acetate 3 hydrate (0.18 g) was added and bromine (60 μl) dissolved in acetic acid (0.5 ml) was dropwise added at 70° C. After cooling, water was added to the reaction mixture and the mixture was neutralized with aqueous ammonia under ice-cooling, extracted with ethyl acetate and dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure and the residue was recrystallized from acetone to give colorless prism crystals (0.21 g, 72.4%), m.p. 156-158° C. (acetone).

Aufarbeitung

  1. additionwas dropwise added at 70° C
  2. temperatureAfter cooling
  3. temperaturecooling
  4. extractionextracted with ethyl acetate
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled away under reduced pressure
  7. customthe residue was recrystallized from acetone

Quellen und Nachweise

ORD-Eintrag
ord-e789c5d0393a40449349d26c8ae6d3d4
Quelldatensatz
uspto-grants-2000_06
Patentnummer
US06080750

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