反应详情

To tert-butyl 4-(2-methyl-4-quinolyl)piperazine-1-carboxylate (4.382 g, 13.38 mmol) was added 40 ml of a 1:1 mixture of dichloromethane and trifluoroacetic acid. The mixture was stirred at room temperature for 15 minutes. The mixture was evaporated to dryness under reduced pressure and the residue dissolved in dichloromethane. The solution was washed with 5% sodium bicarbonate solution and 3M NaOH was added until the aqueous phase remained basic. The phases were separated, the aqueous phase was extracted twice with dichloromethane, the combined organic phases were washed with saturated sodium carbonate solution, water, dried over magnesium sulfate and evaporated to dryness. 2.1 g of a solid were obtained (9.25 mmol, 69%). MS (APCI): m/z=227.8 [M+1]+.

1. customThe mixture was evaporated to dryness under reduced pressure
2. dissolutionthe residue dissolved in dichloromethane
3. washThe solution was washed with 5% sodium bicarbonate solution and 3M NaOH
4. additionwas added until the aqueous phase
5. customThe phases were separated
6. extractionthe aqueous phase was extracted twice with dichloromethane
7. washthe combined organic phases were washed with saturated sodium carbonate solution, water
8. dry with materialdried over magnesium sulfate
9. customevaporated to dryness