反应 #45561

反应方程式

sodium bicarbonate water

2-tert-Butyl-7-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-(3-methoxyphenyl)-5-methyl-1,3-benzoxazole-4-carbonitrile

aluminium chloride

aluminium chloride

→

2-tert-Butyl-7-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-(3-hydroxyphenyl)-5-methyl-1,3-benzoxazole-4-carbonitrile

溶剂

benzene

benzene

反应条件

后处理

1. 1
   洗涤The benzene wash (8.0 ml) of the eggplant-type flask with the starting material adhering
2. 2
   workup.ADDITIONthereto was also added
3. 3
   温度by refluxing for 0.5 hours
4. 4
   温度After cooling
5. 5
   温度under reflux for 15 minutes
6. 6
   温度After cooling
7. 7
   萃取the product was extracted with chloroform (50 ml×2), ethyl acetate (50 ml)

实验过程

2-tert-Butyl-7-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-(3-methoxyphenyl)-5-methyl-1,3-benzoxazole-4-carbonitrile (I-23) (10 mg, 23.1 μmol) was dissolved (partially suspended) in benzene (2.0 ml), and dropwise added to a benzene (2.0 ml) suspension reflux liquid of aluminium chloride (9.2 mg, 69.0 μmol). The benzene wash (8.0 ml) of the eggplant-type flask with the starting material adhering thereto was also added, followed by refluxing for 0.5 hours. After cooling, aluminium chloride (61.7 mg, 462 μmol) was further added, followed by further stirring under reflux for 15 minutes. After cooling, saturated sodium bicarbonate water (50 ml) was added to the reaction liquid, the product was extracted with chloroform (50 ml×2), ethyl acetate (50 ml).

来源