반응 #45752

반응 방정식

Diisopropylethylamine

1-methylpiperazin-2-one hydrochloride

dichloromethane

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

→

compound

수율 99.9%

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

수율 99.9%

용매

Chloroform

반응 조건

후처리

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

실험 절차

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.

출처