Hydrochloric Acid → HCID 178433379, Verbindung

HRID 1617253Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1617253
[SH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][OH:9])=[CH:4][CH:3]=1.[NH2:10][C:11]1[N:16]=[C:15]([OH:17])[C:14](Br)=[C:13]([CH3:19])[N:12]=1.O.Cl>C(O)CO>[NH2:10][C:11]1[N:16]=[C:15]([OH:17])[C:14]([S:1][C:2]2[CH:7]=[CH:6][C:5]([CH2:8][OH:9])=[CH:4][CH:3]=2)=[C:13]([CH3:19])[N:12]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 4677905(4-Sulfanylphenyl)methanolHCID 1784333692-amino-5-bromo-6-methyl-1H-pyrimidin-4-one

Produkt 1

HCID 178433379HCID 178433379, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 174Ethylene GlycolLösungsmittel

Reaktionsbedingungen

Temperatur
155 °C

Versuchsvorschrift

A stirred mixture of (4-mercaptophenyl)methanol (6.72 g), 2-amino-5-bromo-6-methylpyrimidin-4-ol (10.76 g) and K2 CO3 (7.29 g) in ethylene glycol (120 ml) was heated at 155° C. for 9 h. After cooling the mixture was poured into water (500 ml) and neutralised with conc. HCl. The precipitate was filtered, washed with water then 50% EtOH/ether and dried to give the subtitle compound as a solid, 6.7 g. 1H NMR DMSO-d6: δ11.07 (brs, 1H); 7.18 (d, 2H); 6.99 (d, 2H); 6.87 (brs, 2H); 5.09 (s, 1H); 4.41 (s, 2H); 2.24 (s, 3H)

Aufarbeitung

  1. temperatureAfter cooling the mixture
  2. filtrationThe precipitate was filtered
  3. washwashed with water
  4. dry with material50% EtOH/ether and dried

Quellen und Nachweise

ORD-Eintrag
ord-ad4ec7d8ce0644ba867c6d46e99c837c
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08765939B2

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