反应详情

温度

25 °C

Compound 1c (2.25 g; 9 mmol) is suspended in acetonitrile (30 ml) and N,N-diisopropyl ethyl amin (3.03 ml; 17 mmol) is added at 25° C. After 20 min a clear solution is obtained and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride EDCI (2.0 g; 10 mmol) and 1-hydroxybenzotriazole HOBt (1.41 g; 10 mmol) is added. After stirring for 30 min at 25° C. 4-chloroaniline (1.11 g; 9 mmol) is added to the reaction mixture. The mixture is stirred for 18 h at 25° C., evaporated to dryness and dissolved in ethyl acetate (100 ml). The organic phase is washed with 0.1 N HCl (2×100 ml), water and brine and dried over Na2SO4. The organic phase is filtered and the filtrate is evaporated to dryness. Yield: 1.08 g (33.7%), ESI-MS: m/z=368 [M−H]−, Cl-pattern

1. customAfter 20 min a clear solution is obtained
2. stirringThe mixture is stirred for 18 h at 25° C.
3. customevaporated to dryness
4. dissolutiondissolved in ethyl acetate (100 ml)
5. washThe organic phase is washed with 0.1 N HCl (2×100 ml), water and brine
6. dry with materialdried over Na2SO4
7. filtrationThe organic phase is filtered
8. customthe filtrate is evaporated to dryness