Reaktion #597416

ord-c124cd29ea4b4c2b814323dfadb5217d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenthe reaction was concentrated in vacuo

Vorschrift

To the product of Example 110, step a (850 mg, 2.8 mmol) in DCM (14 mL) was added TFA (5 mL). After stirring 2 h, the reaction was concentrated in vacuo. Chromatography on SiO2 eluting with 2 M NH3 in MeOH/DCM afforded the desired product as a pale yellow solid (190 mg, 33%). This material was used without further purification. MS (ESI) mass calcd. C9H10N6, 202.2. m/z found 203.1 [M+H]+. 1H NMR (500 MHz, CDCl3): 8.92 (s, 1H), 8.63 (d, J=1.2 Hz, 1H), 7.85 (d, J=1.2 Hz, 1H), 4.23 (s, 2H), 3.36 (t, J=5.7 Hz, 2H), 3.23 (t, J=5.9 Hz, 2H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09096596B2uspto-grants-2015_08