Reaktion #79088

ord-9735c010b3ba427db4240090948f5867

Reaktionsgleichung

CS(=O)(=O)O
methanesulfonic acid
CC(=O)[O-].N#Cc1c[nH+]c(N)cc1N
2,4-diamino,5-cyanopyridinium acetate
O=CO
formic acid
NCc1ccc(Cl)cc1
4-chlorobenzylamine
CS(=O)(=O)O.Nc1cc2ncnc(NCc3ccc(Cl)cc3)c2cn1
7-Amino-4-(4-chlorobenzylamino)pyrido[4,3-d]pyrimidine Mesylate

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto give a polymesylate salt

Vorschrift

The free base (56 mg, 0.20 mmol)(prepared from 2,4-diamino,5-cyanopyridinium acetate, formic acid and 4-chlorobenzylamine at 200° C. as described in a previous example is precipitated from acetone solution with methanesulfonic acid (105 μL, 0.23 mmol) to give a polymesylate salt. 1H NMR (DMSO) δ 10.59 (1H, t, J=5.6 Hz), 9.24(1H, s), 8.69 (1H, s), 7.42 (4H, s), 6.42 (1H, s), 5.8 (˜6H, vbrs), 4.89 (2H, d, J=5.8 Hz), 2.41 (˜7.5H, s).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06713484B2uspto-grants-2004_03