반응 #2193

반응 방정식

4-chloro-4'-mercaptomethylbenzophenone

ethyl bromide

potassium hydroxide

→

desired product

수율 79.1%

4-Chloro-4'-ethylthiomethylbenzophenone

수율 79.1%

용매

methanol

반응 조건

후처리

1. 1
   온도under reflux
2. 2
   농축concentrated
3. 3
   workup.ADDITIONWater was added to the residue
4. 4
   추출the mixture was extracted with ethyl acetate
5. 5
   세척The ethyl acetate layer was washed with water
6. 6
   건조dried over anhydrous magnesium sulfate
7. 7
   농축concentrated
8. 8
   기타The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1)

실험 절차

4-chloro-4'-mercaptomethylbenzophenone (16.0 g), ethyl bromide (7.4 g) and potassium hydroxide (4.3 g) were added to methanol (250 ml), and the mixture was stirred for 30 minutes under reflux. The reaction mixture was cooled to room temperature and then concentrated. Water was added to the residue, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water and then dried over anhydrous magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1) to obtain the desired product 14.0 g, melting point: 33° to 34° C., yield: 79%).

출처