Methane → HCID 178488765, Verbindung

HRID 280004Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 280004
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([CH2:9][C:10]2[C:15]3[CH:16]=[CH:17][CH2:18][O:19][C:14]=3[C:13]([O:20][CH3:21])=[C:12]([O:22][CH3:23])[CH:11]=2)=[CH:4][N:3]=1.[CH2:24]([OH:35])[C@H:25]([OH:34])[C@H:26]1[O:31][C:29](=[O:30])[C:28]([OH:32])=[C:27]1[OH:33].C>CO>[O:30]=[C:29]1[O:31][C@H:26]([C@H:25]([CH2:24][OH:35])[OH:34])[C:27]([O-:33])=[C:28]1[OH:32].[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([CH2:9][C:10]2[C:15]3[CH:16]=[CH:17][CH2:18][O:19][C:14]=3[C:13]([O:20][CH3:21])=[C:12]([O:22][CH3:23])[CH:11]=2)=[CH:4][N:3]=1

Komponenten

5

Edukt 3

HCID 297MethaneHCID 128497722,4-diamino-5-(7,8-dimethoxy-2H-1-benzopyran-5-ylmethyl)pyrimidineHCID 54670067L-Ascorbic Acid

Produkt 1

HCID 178488765HCID 178488765, VerbindungAusbeute 97,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

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.

Aufarbeitung

  1. filtrationfiltered
  2. customevaporated to dryness
  3. customFurther drying at 40° C. in a vacuum oven

Quellen und Nachweise

ORD-Eintrag
ord-1f719fc921834646813f2d3b3922f158
Quelldatensatz
uspto-grants-1986_05
Patentnummer
US04587342

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