تفاعل #45700

معادلة التفاعل

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

diisopropylethylamine

ethyl azetidine-3-carboxylate hydrochloride

→

Ethyl 1-(4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazol-2-yl)azetidine-3-carboxylate

المذيبات

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter heated
2. 2
   درجة الحرارةunder reflux for 3 hours
3. 3
   غسيلAfter washing with water
4. 4
   تجفيفdrying over anhydrous sodium sulfate
5. 5
   أخرىthe solvent was evaporated away under reduced pressure
6. 6
   أخرىthe resulting residue was purified by silica gel column chromatography (dichloromethane to dichloromethane:methanol=70:1)
7. 7
   أخرىto obtain a brown oil (0.60 g, quant)

الإجراء التجريبي

2-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile (I-130) (0.45 g, 1.57 mmol) was dissolved in dichloromethane (15 ml), then diisopropylethylamine (0.6 ml, 3.53 mmol) and ethyl azetidine-3-carboxylate hydrochloride (I-147) (0.55 g) were added. After heated under reflux for 3 hours, this was diluted with dichloromethane. After washing with water and drying over anhydrous sodium sulfate, the solvent was evaporated away under reduced pressure, and the resulting residue was purified by silica gel column chromatography (dichloromethane to dichloromethane:methanol=70:1) to obtain a brown oil (0.60 g, quant).

المصدر