반응 #2199669

반응 방정식

sodium hydride

(2-amino-4,5-difluorophenyl)-(2-chlorophenyl)-methanone

4-morpholinepropanol

→

(2-amino-5-fluoro-4-(3-(4-morpholinyl)propoxy)phenyl)-(2-chlorophenyl)-methanone

수율 64.9%

용매

dioxane

반응 조건

후처리

1. 1
   기타The mixture was quenched by the addition of 50 mL of water
2. 2
   추출The mixture was extracted with ethyl acetate
3. 3
   세척the extract washed with water
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   여과filtered
6. 6
   농축concentrated under reduced pressure
7. 7
   기타The residue was triturated with hexane
8. 8
   기타recrystallized from hexane-ethyl acetate

실험 절차

A mixture of 1.4 g (0.035 mole) of 60% sodium hydride, 25 mL of dioxane, 2.68 g (0.01 mole) of (2-amino-4,5-difluorophenyl)-(2-chlorophenyl)-methanone (Xmm) and 2.23 g (0.016 mole) of 4-morpholinepropanol was stirred at room temperature for 4 hours. The mixture was quenched by the addition of 50 mL of water. The mixture was extracted with ethyl acetate, and the extract washed with water, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The residue was triturated with hexane and then recrystallized from hexane-ethyl acetate to give 2.55 g of (2-amino-5-fluoro-4-(3-(4-morpholinyl)propoxy)phenyl)-(2-chlorophenyl)-methanone (Xi). MH+/Z=393.

출처