[Sn](Cl)Cl.[Cl:4][C:5]1[C:6]([F:15])=[C:7]([N+:12]([O-])=O)[CH:8]=[CH:9][C:10]=1[F:11].Cl.[OH-].[Na+]>O.C(OCC)C>[Cl:4][C:5]1[C:6]([F:15])=[C:7]([CH:8]=[CH:9][C:10]=1[F:11])[NH2:12]135 g of tin(II) chloride (dihydrate) was added in small fractions to a stirred suspension of 23 g of 3-chloro-2,4-difluoronitrobenzene in 110 cm3 of a 37% aqueous hydrochloric acid solution and 25 cm'of diethyl ether. After the addition, the mixture was heated for 30 minutes at a temperature in the region of 40° C. After cooling the reaction mass, the mixture was poured over 300 cm3 of water supplemented with 150 g of ice. The mixture was made highly alkaline by addition of caustic soda, and then extracted twice with 250 cm3 of chloroform. The extracts were combined, dried over magnesium sulphate, and then concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C. 17.4 g of 3-chloro-2,4-difluoroaniline was obtained in the form of a beige solid, which melted at 58° C.
Wird geladen…
