6-bromohexan-1-amine;hydrobromide

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A suspension of 4-[3-chlorosulfonylphenylazo]-1-ethoxycarboxy-5-methanesulfonamidonaphthalene (20.4 g), 6-bromohexylamine hydrobromide (14.4 g), 2,6-lutidine (600 ml) and tetrahydrofuran (30 ml) was reacted for one hour at 50°-55° C. The mixture was cooled and filtered; the filtrate was concentrated to an oil which was dissolved in a minimum amount of acetonitrile and chromatographed on silica gel using acetonitrile as the eluant. The orange colored eluate was concentrated and cooled to obtain the product; yield 7.3 g (32%), m.p. 163°-5° C. was reacted for one hour at 50°-55° C The mixture was cooled filtered the filtrate was concentrated to an oil which was dissolved in a minimum amount of acetonitrile chromatographed on silica gel The orange colored eluate was concentrated cooled to obtain the product

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A suspension of 4-(4-chlorosulfonylphenylazo)-5-hydroxy-3-methylcarbamoyl-1-phenyl-1H-pyrazole (12 g) and 6-bromohexylamine hydrobromide (12 g) in 2,6-lutidine (300 ml) and di-isopropylethylamine (3 ml) was allowed to react for 18 hours at room temperature. The reaction mixture was filtered; the filtrate was concentrated to yield an oily material which was washed with hot water to yield the above-identified pyrazole derivative; yield 7.4 g (44%), m.p. 234°-236° C. to react for 18 hours at room temperature The reaction mixture was filtered the filtrate was concentrated to yield an oily material which was washed with hot water