Bromine → 2-Amino-3-bromo-5-methylpyrazine

HRID 361413Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 361413
[Br:1]Br.[NH2:3][C:4]1[CH:9]=[N:8][C:7]([CH3:10])=[CH:6][N:5]=1>C(Cl)(Cl)Cl>[NH2:3][C:4]1[C:9]([Br:1])=[N:8][C:7]([CH3:10])=[CH:6][N:5]=1

Komponenten

4

Edukt 2

HCID 24408BromineHCID 3132155-Methylpyrazin-2-amine

Produkt 1

HCID 98990432-Amino-3-bromo-5-methylpyrazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

A solution of bromine (0.11 ml) in chloroform (20 ml) was added dropwise over 20 minutes to a solution of 2-amino-5-methylpyrazine (0.218 g) in chloroform (30 ml) which was protected from light. The reaction mixture was stirred for 90 minutes after addition was complete and was then washed with water (50 ml). The organic phase was dried (MgSO4) and volatile material was removed by evaporation to give a yellow oil. The oil was purified by elution with dichloromethane through a silica gel Mega Bond Elut column to give 2-amino-3-bromo-5-methylpyrazine (0.286 g) as a white solid, m.p. 51°-52° C.; mass spectrum (+ve CI): 188 (M+H)+.

Aufarbeitung

  1. additionafter addition
  2. washwas then washed with water (50 ml)
  3. dry with materialThe organic phase was dried (MgSO4) and volatile material
  4. customwas removed by evaporation
  5. customto give a yellow oil
  6. customThe oil was purified by elution with dichloromethane through a silica gel Mega Bond Elut column

Quellen und Nachweise

ORD-Eintrag
ord-13e1cd739e3b4ec59ea400f3adfb8c5f
Quelldatensatz
uspto-grants-1999_02
Patentnummer
US05866568

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