3-氯-4氟硫酚

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Iodomethane (1.15 ml) was added to a stirred mixture of 3-chloro-4-fluoro-benzenethiol (3.0 g) and potassium carbonate (2.48 g) in DMF (20 ml) and left overnight. The reaction was diluted with water and extracted with diethylether, the organics were dried and evaporated under reduced pressure, yield 4.3 g. extracted with diethylether the organics were dried evaporated under reduced pressure, yield 4.3 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Iodomethane (1.15 ml) was added to a stirred mixture of 3-chloro-4-fluoro-benzenethiol (3.0 g) and potassium carbonate (2.48 g) in DMF (20 ml) and left overnight. The reaction was diluted with water and extracted with diethylether, the organics were dried and evaporated under reduced pressure, yield 4.3 g. extracted with diethylether the organics were dried evaporated under reduced pressure, yield 4.3 g

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Iodomethane (1.15 ml) was added to a stirred mixture of 3-chloro-4-fluoro-benzenethiol (3.0 g), potassium carbonate (2.48 g) in DMF (20 ml) and left overnight. The reaction was diluted with water and extracted with diethylether, the organics were dried and evaporated under reduced pressure, yield 4.3 g. extracted with diethylether the organics were dried evaporated under reduced pressure, yield 4.3 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The thiophenol from the preceding experiment (34.5 g) is added at 50° C. to a solution of potassium hydroxide (40 g) in water (425 ml) and this mixture is stirred until it becomes homogeneous. Then, o-iodophenylacetic acid (55.0 g) and copper powder (2.0 g) are added and the mixture refluxed for 24 hours. While still warm, the solution is filtered with charcoal, the filtrate diluted with water and acidified with hydrochloric acid. The separated crude oily acid is extracted with benzene, the solvent evaporated and the residue crystallized from aqueous ethanol, yielding 45.2 g (72%) of 2-(3-chloro-4-fluorophenylthio)phenylacetic acid which in the pure state melts at 85°-87° C. (cyclohexane-hexane). the mixture refluxed for 24 hours While still warm the solution is filtered with charcoal the filtrate diluted with water The separated crude oily acid is extracted with benzene the solvent evaporated the residue crystallized from aqueous ethanol