Reaktion #62722

ord-48cd5ce1833a474c94a5f8f0bde048e8

Reaktionsgleichung

COc1cc(Cc2cnc(N)nc2N)c2c(c1OC)OCC=C2
2,4-diamino-5-(7,8-dimethoxy-2H-1-benzopyran-5-ylmethyl)pyrimidine
O=C1O[C@H]([C@@H](O)CO)C(O)=C1O
(+)-ascorbic acid
C
charcoal
COc1cc(Cc2cnc(N)nc2N)c2c(c1OC)OCC=C2.O=C1O[C@H]([C@@H](O)CO)C([O-])=C1O
title compound
Ausbeute 97.4%
COc1cc(Cc2cnc(N)nc2N)c2c(c1OC)OCC=C2.O=C1O[C@H]([C@@H](O)CO)C([O-])=C1O
2,4-Diamino-5-(7,8-dimethoxy-2H-1-benzopyran-5-ylmethyl)pyrimidine Ascorbate
Ausbeute 97.4%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationfiltered
  2. 2
    Sonstigeevaporated to dryness
  3. 3
    SonstigeFurther drying at 40° C. in a vacuum oven

Vorschrift

To 2,4-diamino-5-(7,8-dimethoxy-2H-1-benzopyran-5-ylmethyl)pyrimidine (5.00 g, 15.9 mmol) in 450 mL of boiling methanol was added a solution of L (+)-ascorbic acid (2.80 g, 15.9 mmol) in 50 mL of methanol. The solution was treated with charcoal, filtered, and evaporated to dryness. Further drying at 40° C. in a vacuum oven gave 7.58 g (97.2%) of the title compound. Anal. Calcd for C16H18H4O3.C6H8O6.H2O: C, 51.97; H, 5.55; N, 11.02. Found: C, 51.95; H, 5.57; N, 11.02.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04761475uspto-grants-1988_08