반응 #45561

반응 방정식

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

용매

benzene

benzene

반응 조건

후처리

1. 1
   세척The benzene wash (8.0 ml) of the eggplant-type flask with the starting material adhering
2. 2
   workup.ADDITIONthereto was also added
3. 3
   온도by refluxing for 0.5 hours
4. 4
   온도After cooling
5. 5
   온도under reflux for 15 minutes
6. 6
   온도After cooling
7. 7
   추출the product was extracted with chloroform (50 ml×2), ethyl acetate (50 ml)

실험 절차

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).

출처