Reaktion #1599269

ord-5a76c5ed776b46ed9edc167c0c3af0be

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with 1N NaOH (3×200 mL) and NaCl(sat.) (100 mL)
  2. 2
    Trocknendried over Na2SO4
  3. 3
    Filtrationfiltered
  4. 4
    Einengenconcentrated

Vorschrift

To a solution of 4-methylpyrimidine-2-ylamine (10.9 g, 100 mmol) in chloroform (400 mL) was added N-bromosuccinimide (17.8 g, 100 mmol). The solution was stirred in the dark for 15 hours, at which time it was added to CH2Cl2 (1400 mL), washed with 1N NaOH (3×200 mL) and NaCl(sat.) (100 mL), dried over Na2SO4, filtered and concentrated, yielding 5-bromo-4-methylpyrimidine-2-ylamine (18.8 g, 99%). LCMS (m/z): 188.0/190.0 (MH+). 1H NMR (CDCl3): δ 8.22 (s, 1H), 5.02 (bs, 2H), 2.44 (s, 3H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08217035B2uspto-grants-2012_07