Phosphorus oxychloride → 5-Chloro-7-[2,4-dichlorophenyl][1,2,4]triazolo[1,5-c]pyrimidine

HRID 2171554Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2171554
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:14]=[C:13](O)[N:12]2[N:16]=[CH:17][N:18]=[C:11]2[CH:10]=1.P(Cl)(Cl)([Cl:21])=O>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1>[Cl:21][C:13]1[N:12]2[N:16]=[CH:17][N:18]=[C:11]2[CH:10]=[C:9]([C:3]2[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=2[Cl:1])[N:14]=1

Komponenten

4

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 178517485HCID 178517485, Verbindung

Produkt 1

HCID 593130895-Chloro-7-[2,4-dichlorophenyl][1,2,4]triazolo[1,5-c]pyrimidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 66133Benzyl triethylammonium chlorideKatalysator

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

2.07 g (7.4 mmol) of 7-[2,4-dichlorophenyl][1,2,4]triazolo[1,5-c]pyrimidin-5-ol (Example 137A) are introduced into phosphoryl chloride (20 ml), 5.0 g (22 mmol) of benzyltriethylammonium chloride are added, and the reaction mixture is stirred at 120° C. for 16 h. The reaction mixture is concentrated and cautiously poured onto ice, while stirring vigorously, and the mixture is stirred for 10 min. The solid is filtered off with suction. 1100 mg (50% of theory) of the product are obtained.

Aufarbeitung

  1. additionare added
  2. concentrationThe reaction mixture is concentrated
  3. additioncautiously poured onto ice
  4. stirringwhile stirring vigorously
  5. stirringthe mixture is stirred for 10 min
  6. filtrationThe solid is filtered off with suction
  7. custom1100 mg (50% of theory) of the product are obtained

Quellen und Nachweise

ORD-Eintrag
ord-23e2d654830b43d289e6196e8dbe3f19
Quelldatensatz
uspto-grants-2015_06
Patentnummer
US09051323B2

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