Reaktion #45752

Reaktionsgleichung

Diisopropylethylamine

1-methylpiperazin-2-one hydrochloride

dichloromethane

2-chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile

→

compound

Ausbeute 99.9%

7-Fluoro-5-methyl-2-(4-methyl-3-oxopiperazin-1-yl)-6-phenyl-1,3-benzoxazole-4-carbonitrile

Ausbeute 99.9%

Lösungsmittel

Chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenby washing with saturated brine (50 ml)
2. 2
   TrocknenAfter drying over anhydrous sodium sulfate and concentration under reduced pressure
3. 3
   Sonstigethe resulting residue was purified by silica gel column chromatography (eluent, chloroform:methanol=20:1)

Vorschrift

Diisopropylethylamine (232 μl, 1.36 mmol) and 1-methylpiperazin-2-one hydrochloride (103 mg, 0-682 mmol) were added to a dichloromethane (6 ml) solution of 2-chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile (I-130) (163 mg, 0.569 mmol), followed by stirring at room temperature for 30 minutes. Chloroform (50 ml) was added to the reaction liquid, followed by washing with saturated brine (50 ml). After drying over anhydrous sodium sulfate and concentration under reduced pressure, the resulting residue was purified by silica gel column chromatography (eluent, chloroform:methanol=20:1) to obtain the entitled compound (207 mg, 99.9%) as a colorless solid.

Quelle