反应详情

A mixture of trifluoroacetic acid (0.5 mL, 0.15 mmol) and tert-butyl 4-((4-(3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)piperazin-1-yl)methyl)phenylcarbamate (0.072 g, 0.15 mmol) in dichloromethane (2 mL) was stirred at ambient temperature for 2 hours and then evaporated to give an involatile residue. The residue was purified by hplc using a Phenomenex Luna C18 100A column (10μ silica, 21 mm diameter, 150 mm length) eluted with decreasingly polar mixtures of water (containing 0.1% TFA) and acetonitrile as eluents to give a partially purified product that was further purified by ion exchange chromatography using an SCX column eluted 7M aquous ammonia in methanol to give 4-((4-(3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)piperazin-1-yl)methyl)aniline (0.032 g, 56.2%) as a white solid.

1. customevaporated
2. customto give an involatile residue
3. customThe residue was purified by hplc
4. washeluted with decreasingly polar mixtures of water (containing 0.1% TFA) and acetonitrile as eluents
5. customto give a partially purified product that
6. customwas further purified by ion exchange chromatography
7. washeluted 7M aquous ammonia in methanol