反应详情

20 ml of thionyl chloride is added to 11.82 g (0.04 mol) of 3-bromo-5-chloro-2,6-dimethoxybenzoic acid. The mixture is heated on a steam bath for 1 hour. To the solution is added 50 ml of toluene. The solvent and excess thionyl chloride is evaporated at reduced pressure. The residue is dissolved in 50 ml of dry methyl ethyl ketone. The solution is added dropwise while stirring to 5.13 g (0.04 mol) 2-(aminomethyl)-1-ethylpyrrolidine in 50 ml methyl ethyl ketone. After stirring for 30 minutes at room temperature 300 ml of ether is added. The obtained semisolid product is separated and dissolved in 300 ml of water. Sodium hydroxide solution is added while stirring and cooling in ice. The precipitate is collected and washed with water. Yield: 12.0 g, m.p. 124°-25° C.

1. temperatureThe mixture is heated on a steam bath for 1 hour
2. customThe solvent and excess thionyl chloride is evaporated at reduced pressure
3. dissolutionThe residue is dissolved in 50 ml of dry methyl ethyl ketone
4. additionThe solution is added dropwise
5. additionis added
6. customThe obtained semisolid product is separated
7. dissolutiondissolved in 300 ml of water
8. additionSodium hydroxide solution is added
9. temperaturecooling in ice
10. customThe precipitate is collected
11. washwashed with water