반응 #1573901

반응 방정식

4-chloro-N-(3-[1,3]dioxolan-2-yl-phenyl)-benzamide

HCl

→

title compound

수율 84.4%

4-Chloro-N-(3-formyl-phenyl)-benzamide

수율 84.4%

용매

ethyl acetate

1,4-dioxane

반응 조건

후처리

1. 1
   기타The organic phase is separated
2. 2
   추출the aqueous phase is extracted twice with ethyl acetate (100 mL)
3. 3
   세척The combined organic phases are washed with brine (200 mL)
4. 4
   건조dried over MgSO4
5. 5
   기타After evaporation of the organic solvents the residue
6. 6
   기타is triturated with diethyl ether

실험 절차

A solution of 4-chloro-N-(3-[1,3]dioxolan-2-yl-phenyl)-benzamide (14.33 g, 47.2 mmol) in 1,4-dioxane (120 mL) is treated with 1N aq. HCl (120 mL) at RT for 1 h then at 60° C. for 30 min. The reaction mixture is cooled down to RT and diluted with ethyl acetate (100 mL). The organic phase is separated and the aqueous phase is extracted twice with ethyl acetate (100 mL). The combined organic phases are washed with brine (200 mL) and dried over MgSO4. After evaporation of the organic solvents the residue is triturated with diethyl ether to give the title compound (10.34 g, 84%) as a beige powder; LC-MS B: tR=0.83 min; [M+H]+=259.82.

출처