Reaktion #78185

Reaktionsgleichung

2-acetyl-5-aminophenol

1-chloro-4-(4-pyridylmethyl)phthalazine

NH3

dichloromethane

→

title compound

(4-Acetyl-3-hydroxyanilino)-4-(4-pyridylmethyl)phthalazine

Lösungsmittel

DMEU

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeare heated for 3-18 h to 100° C
2. 2
   Filtrationfiltered via Celite
3. 3
   TrocknenThe organic phase of the filtrate is dried (Na2SO4)
4. 4
   Sonstigeevaporated
5. 5
   Sonstigechromatographed
6. 6
   Sonstige(SiO2; ethyl acetate/CH3OH, 40:1→10:1) Crystallization from acetonitrile

Vorschrift

302 mg (2.0 mmol) 2-acetyl-5-aminophenol (Maybridge) and 256 mg (1.00 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine (Example 67A.1) in 2 ml DMEU are heated for 3-18 h to 100° C. The reaction mixture is stirred with 10 ml NH3 solution (10% in water) and 25 ml ethyl actetate (or dichloromethane) and filtered via Celite. The organic phase of the filtrate is dried (Na2SO4), evaporated, and chromatographed (SiO2; ethyl acetate/CH3OH, 40:1→10:1) Crystallization from acetonitrile yields the title compound: m.p.: 234-236° C.; HPLC: tRet(Grad5-40)=9.5; FAB MS (M+H)+=371.

Quelle