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With n-butyllithium; In tetrahydrofuran; hexane; water; ethyl acetate;
REFERENCE EXAMPLE 75 To a solution of <strong>[33786-89-9]5-chloro-1,3-benzenediamine</strong> (7.48 g) in tetrahydrofuran (50 ml) was added slowly a 1.5M solution of n-butyl lithium in n-hexane (27.3 ml) at 0° C. The resultant mixture was stirred for 30 minutes at 0° C. To the mixture was added a solution of 3-chloro-6-fluorobenzo[d]isoxazole (1.8 g) in tetrahydrofuran (5 ml). After stirring for 15 minutes at 0° C. and for an hour at ambient temperature, the reaction mixture was poured into a mixture of water and ethyl acetate. The separated organic layer was washed well with 1N-hydrochloric acid and dried over potassium carbonate. After evaporation under reduced pressure, the residue was crystallized from methanol to give 5-chloro-N-(6-fluorobenzo[d]isoxazol-3-yl)benzene-1,3-diamine (1.54 g). APCI-Mass: 278 (m/z, (M+H)+) NMR(DMSO-d6, delta): 5.50(2H, s), 6.24(1H, t, J=3.7 Hz), 6.88(2H, t, J=1.9 Hz), 7.27(1H, dt, J=2.1, 9.0 Hz), 7.57(1H, dd, J=2.1, 9.0 Hz), 8.09-8.22(1H, m), 9.47(1H, s).
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