反应 #1328421

ord-284ab8b931e540ada41736c24d6676e3

反应方程式

O=C([O-])[O-].[K+].[K+]
potassium carbonate
O=C(O)CCBr
3-bromopropionic acid
COC(=O)c1ccc(Cl)cc1S
methyl 2-mercapto-4-chlorobenzoate
COC(=O)c1ccc(Cl)cc1SCCC(=O)O
Methyl 2-(2-hydroxycarbonyleth-1-yl)thio-4-chlorobenzoate

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.DISTILLATIONThe solvent was distilled off
  2. 2
    萃取the mixture was extracted with diethyl ether
  3. 3
    过滤the resulting precipitate was filtered off with suction
  4. 4
    其他dried

实验过程

179.5 g (1.3 mol) of potassium carbonate and, a little at a time, 94.5 g (0.62 mol) of 3-bromopropionic acid were added to a solution of 125.4 g (0.62 mol) of methyl 2-mercapto-4-chlorobenzoate in 1.5 l of acetone, and the reaction mixture was stirred at room temperature for 12 hours. The solvent was distilled off, the residue was taken up in water and the mixture was extracted with diethyl ether. The aqueous phase was then made acidic using concentrated hydrochloric acid, and the resulting precipitate was filtered off with suction and dried. This gave 150 g (88%) of methyl 2-(2-hydroxycarbonyleth-1-yl)thio-4-chlorobenzoate.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07115545B1uspto-grants-2006_10