Dimethylformamide → HCID 18706853, Verbindung

HRID 1421875Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1421875
[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]=[C:4]([Cl:16])[N:3]=1.[Cl:17]N1C(=O)CCC1=O.CN(C)C=O>C(OCC)(=O)C>[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]([Cl:17])=[C:4]([Cl:16])[N:3]=1

Komponenten

5

Edukt 3

HCID 6228DimethylformamideHCID 31398ChlorosuccinimideHCID 385223HCID 385223, Verbindung

Produkt 1

HCID 18706853HCID 18706853, VerbindungAusbeute 54,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To 2-amino-6-chloro-4-[[(1-hydroxymethyl-1-cyclobutyl)methyl]amino]pyrimidine (0.24 g, 2.0 mmol) were added N-chlorosuccinimide (0.27 g, 2.0 mmol) and dimethylformamide (1.5 ml), and the mixture was stirred at room temperature for 2 days. Ethyl acetate was added and the mixture was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure and the residue was purified by silica gel column chromatography (chloroform:methanol=100:1) to give colorless prism crystals (0.3 g, 54.2%), m.p. 179-181° C. (acetone).

Aufarbeitung

  1. washthe mixture was washed with water
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled away under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (chloroform:methanol=100:1)

Quellen und Nachweise

ORD-Eintrag
ord-225cb617e10e4cb4ba5b09eccd0edbd6
Quelldatensatz
uspto-grants-2000_06
Patentnummer
US06080750

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