反应 #2193

ord-854622046616431a8dec648c46bb4905

反应方程式

O=C(c1ccc(Cl)cc1)c1ccc(CS)cc1
4-chloro-4'-mercaptomethylbenzophenone
CCBr
ethyl bromide
[K+].[OH-]
potassium hydroxide
CCSCc1ccc(C(=O)c2ccc(Cl)cc2)cc1
desired product
收率 79.1%
CCSCc1ccc(C(=O)c2ccc(Cl)cc2)cc1
4-Chloro-4'-ethylthiomethylbenzophenone
收率 79.1%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度under reflux
  2. 2
    浓缩concentrated
  3. 3
    workup.ADDITIONWater was added to the residue
  4. 4
    萃取the mixture was extracted with ethyl acetate
  5. 5
    洗涤The ethyl acetate layer was washed with water
  6. 6
    干燥dried over anhydrous magnesium sulfate
  7. 7
    浓缩concentrated
  8. 8
    其他The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1)

实验过程

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%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05728699uspto-grants-1998_03