[NH2:1][C:2]1[C:3]([F:18])=[CH:4][C:5]([Cl:17])=[C:6]([N:8]([S:12]([CH2:15][Cl:16])(=[O:14])=[O:13])C(=O)C)[CH:7]=1.Cl>C(O)C.[OH-].[Na+]>[NH2:1][C:2]1[C:3]([F:18])=[CH:4][C:5]([Cl:17])=[C:6]([NH:8][S:12]([CH2:15][Cl:16])(=[O:14])=[O:13])[CH:7]=13 g (0.0095 mol) of N-(5-amino-2-chloro-4-fluorophenyl)-N[(chloromethyl)sulfonyl]acetamide were dissolved in 30 mL of ethanol and 30 mL of 25% sodium hydroxide solution. The mixture was stirred for 3 hours at 50° C. and then cooled to room temperature. 6 N hydrochloric acid was added with stirring and cooling until the solution had a pH of 5-6. The suspension was further cooled to 0-5° C., filtered, washed with water and dried to yield 2.4 g (92%) of the title compound as a solid melting at 103.5-105.5° C. Recrystallization from toluene raised the melting point to 105-106° C.
読み込み中…
