5-Amino-2,4-dichloropyrimidine → 5-Amino-2-chloro-4-methylthiopyrimidine

HRID 343379Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 343379
[CH3:1][S-:2].[Na+].[NH2:4][C:5]1[C:6](Cl)=[N:7][C:8]([Cl:11])=[N:9][CH:10]=1>CO>[NH2:4][C:5]1[C:6]([S:2][CH3:1])=[N:7][C:8]([Cl:11])=[N:9][CH:10]=1

Komponenten

4

Edukt 2

HCID 2577975-Amino-2,4-dichloropyrimidineHCID 4378561Sodium methanethiolate

Produkt 1

HCID 187048095-Amino-2-chloro-4-methylthiopyrimidineAusbeute 35 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Sodium methanethiolate (0.342 g) was added to a solution of 5-amino-2,4-dichloropyrimidine (1 g) in methanol (5 ml) and the mixture was heated at reflux for 2 hours. Volatile material was then removed by evaporation and water (1 ml) was added. The suspended solid was collected by filtration, washed with hexane (10 ml) and dried under vacuum to give 5-amino-2-chloro-4-methylthiopyrimidine (0.3 g); 1H NMR (CDCl3): 2.55 (s, 3H), 7.75 (s, 1H); mass spectrum (+ve CI): 175 (M+H)+.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 2 hours
  3. customVolatile material was then removed by evaporation and water (1 ml)
  4. additionwas added
  5. filtrationThe suspended solid was collected by filtration
  6. washwashed with hexane (10 ml)
  7. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-de8bf311c65c46e2a5e7d32fa106cf0d
Quelldatensatz
uspto-grants-1999_01
Patentnummer
US05861401

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