反应详情

A solution of 0.271 g (1.236 mmol) of (3-(2,4-dichloro-phenyl)-propionic acid in 3.00 mL thionyl chloride was stirred for 2 hours at RT, evaporated down i. vac. and dissolved in 10 mL dichloromethane. This solution of the acid chloride was slowly added dropwise, while cooling with ice, to a solution of 0.300 (1.236 mmol) of 3-chloro-4-(2-diethylamino-ethoxy)-phenylamine (intermediate product Z1b) and 0.32 mL (1.854 mmol) of ethyl-diisopropylamine in 10 mL dichloromethane and the mixture was stirred for 16 hours at RT. The reaction mixture was washed with sat. aqueous sodium bicarbonate solution, dried over magnesium sulphate and evaporated down i. vac. The residue was dissolved in EtOAc and purified by column chromatography (silica gel, EtOAc/MeOH/conc. aqueous ammonia 90:10:1).

1. customevaporated down i
2. dissolutionand dissolved in 10 mL dichloromethane
3. additionThis solution of the acid chloride was slowly added dropwise
4. washThe reaction mixture was washed with sat. aqueous sodium bicarbonate solution
5. dry with materialdried over magnesium sulphate
6. customevaporated down i
7. dissolutionThe residue was dissolved in EtOAc
8. custompurified by column chromatography (silica gel, EtOAc/MeOH/conc. aqueous ammonia 90:10:1)