反应详情

The solution of 13.1 g of 2,5-difluorothiophenol (I.Cervena et al., Collect. Czech. Chem. Commun. 45, 2688, 1980) in 20 ml hexamethylphosphortriamide is treated with a solution of 3.6 g of sodium hydroxide in 6 ml of water and then with 13.65 g of 2,5-dichlorobenzaldehyde (of Example 6, reference above). Then, the mixture is heated while stirring for 5.5 hours to 100° C. It is then diluted with 150 ml of water and extracted with benzene. The extract is washed with a 5% sodium hydroxide solution and water, dried with magnesium sulfate and evaporated. The residue is crystallized from a mixture of benzene and petroleum ether. There are obtained 16.4 g (74%) 2-(2,5-difluorophenylthio)-5-chlorobenzaldehyde which melts in a pure state at 88°-90° C.

1. temperatureThen, the mixture is heated
2. extractionextracted with benzene
3. washThe extract is washed with a 5% sodium hydroxide solution and water
4. dry with materialdried with magnesium sulfate
5. customevaporated
6. customThe residue is crystallized from a mixture of benzene and petroleum ether