6-chloro-N4-o-tolylpyrimidine-4,5-diamine → HCID 57438664, Verbindung

HRID 1098226Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1098226
[N:1]([O-])=O.[Na+].[Cl:5][C:6]1[N:11]=[CH:10][N:9]=[C:8]([NH:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[CH3:19])[C:7]=1[NH2:20]>C(O)(=O)C.C(Cl)Cl>[Cl:5][C:6]1[C:7]2[N:20]=[N:1][N:12]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[CH3:19])[C:8]=2[N:9]=[CH:10][N:11]=1

Komponenten

5

Edukt 2

HCID 234775416-chloro-N4-o-tolylpyrimidine-4,5-diamineHCID 23668193Sodium Nitrite

Produkt 1

HCID 57438664HCID 57438664, VerbindungAusbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Sodium nitrite (0.323 g, 4.69 mmol) was added to 6-chloro-N4-o-tolylpyrimidine-4,5-diamine (Intermediate AP5)(1 g, 4.26 mmol) in acetic acid (50% Aq) (25 mL)and DCM (25 mL) at room temperature. The resulting solution was stirred at room temperature for 15 minutes. The reaction mixture was separated and the organic phase was washed with water (10 mL), dried (MgSO4) and evaporated to give crude 7-chloro-3-o-tolyl-3H-[1,2,3]triazolo[4,5-d]pyrimidine (0.980 g, 94%) that was used without further purification.

Aufarbeitung

  1. customThe reaction mixture was separated
  2. washthe organic phase was washed with water (10 mL)
  3. dry with materialdried (MgSO4)
  4. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-0ef68f50d3a0490db7537973997e3a39
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08143263B2

Notizen zur Reaktion

Wird geladen…