Hydrogen Bromide → HCID 68577349, Verbindung

HRID 2046423Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2046423
C(OC(=O)[NH:10][CH2:11][CH2:12][C:13]1[N:14]([CH3:26])[C:15](=[O:25])[CH:16]=[C:17]([C:19]2[CH:24]=[CH:23][N:22]=[CH:21][N:20]=2)[N:18]=1)C1C=CC=CC=1.Br>C(O)(=O)C>[NH2:10][CH2:11][CH2:12][C:13]1[N:14]([CH3:26])[C:15](=[O:25])[CH:16]=[C:17]([C:19]2[CH:24]=[CH:23][N:22]=[CH:21][N:20]=2)[N:18]=1

Komponenten

4

Edukt 2

HCID 260Hydrogen BromideHCID 25117356HCID 25117356, Verbindung

Produkt 1

HCID 68577349HCID 68577349, VerbindungAusbeute 76,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

1.43 g (3.93 mmol) of [2-(1-methyl-6-oxo-1,6-dihydro-[4,4′]bipyrimidinyl-2-yl)-ethyl]-carbamic acid benzyl ester was dissolved in 4.43 g (31.44 mmol) of hydrobromide acid in acetic acid. The mixture was stirred at room temperature for 2 h and concentrated in vacuo. The resulting precipitate was dissolved in water, basified with an aqueous solution of sodium hydroxide (30%) and extracted with a mixture of dichloromethane/methanol/aqueous ammonia solution (29%) in the proportions 80/20/2. The combined extracts were dried over anhydrous sodium sulfate and concentrated in vacuo to give 0.693 g of a white powder.

Aufarbeitung

  1. concentrationconcentrated in vacuo
  2. dissolutionThe resulting precipitate was dissolved in water
  3. extractionextracted with a mixture of dichloromethane/methanol/aqueous ammonia solution (29%) in the proportions 80/20/2
  4. dry with materialThe combined extracts were dried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-1a0e6281fb564302a2b1c7bd7e39d504
Quelldatensatz
uspto-grants-2013_11
Patentnummer
US08592437B2

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