[CH3:1][N:2]1[C:6]([O:7][C:8]2[CH:13]=[C:12]([CH3:14])[CH:11]=[C:10]([O:15]C3N(C)N=C(C(F)(F)F)C=3)[N:9]=2)=[CH:5][C:4]([C:26]([F:29])([F:28])[F:27])=[N:3]1.[OH-].[Na+].Cl>CS(C)=O.O.CCCCC.C(OCC)(=O)C>[OH:15][C:10]1[N:9]=[C:8]([O:7][C:6]2[N:2]([CH3:1])[N:3]=[C:4]([C:26]([F:29])([F:28])[F:27])[CH:5]=2)[CH:13]=[C:12]([CH3:14])[CH:11]=1
A mixture of 2,6-bis(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methylpyridine (prepared according to WO 94/22833; 4.2 g, 10 mmol) and NaOH (1 g, 25 mmol) is heated in DMSO (50 ml) and water (5 ml) for 36 h at 100° C. After cooling, the reaction mixture is diluted with water and acidified with hydrochloric acid. The mixture is diluted with pentane/ethyl acetate (300 ml by volume ration 1/1) and the organic layer is washed 6 times with water. The organic layer is dried with anhydrous magnesium sulfate, filtered and evaporated in vacuo. Purification by flash chromatography (silica gel: pentane/ethyl acetate 8/2 v/v and 7/3 v/v) yields the title compound (1.9 g, 70% yield) of m.p. 159° C.
Wird geladen…
