Reaktion #722832

ord-758e8aa6c8224b5ab6ae61b4ec32612b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThis compound was prepared
  2. 2
    SonstigeThe crude material was purified by flash chromatography on silica gel with 20:1 CHCl3

Vorschrift

This compound was prepared according to the method described in Example 2 by employing 4-chloro-2-methyl-6-phenylpyrrolo[3,2-d]pyrimidine (Example 1(e)) (70 mg, 0.287 mmol), pyrrolidine (Aldrich Chemical Company) (0.12 mL, 1.44 mmol) and K2CO3 (0.397 g, 2.87 mmol) in H2O (2 mL). The crude material was purified by flash chromatography on silica gel with 20:1 CHCl3:MeOH as eluant to give 42.1 mg (53%) of the title compound as an off-white solid. An analytical sample was obtained by recrystallization from EtOH. 1H NMR (CDCl3; 500 MHz): δ 2.07 (t, 4, J=6.3), 2.58 (s, 3), 3.88-3.90 (m, 4), 6.71 (s, 1), 7.36-7.46 (m, 3), 7.63 (d, 2, J=7.7). MS m/z: 279.5 (M+1), 277.5 (M−1). HRMS: Calcd for M+H: 279.1610. Found: 279.1613.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06187777B1uspto-grants-2001_02