反应 #45700

反应方程式

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

溶剂

dichloromethane

dichloromethane

反应条件

后处理

1. 1
   温度After heated
2. 2
   温度under reflux for 3 hours
3. 3
   洗涤After washing with water
4. 4
   干燥drying over anhydrous sodium sulfate
5. 5
   其他the solvent was evaporated away under reduced pressure
6. 6
   其他the resulting residue was purified by silica gel column chromatography (dichloromethane to dichloromethane:methanol=70:1)
7. 7
   其他to obtain a brown oil (0.60 g, quant)

实验过程

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).

来源