반응 #427649

반응 방정식

5-bromopyridin-2,3-diol

Dibromomethane

cesium carbonate

DMF

→

5-bromo-[1,3]dioxolo[4,5-b]pyridine

수율 13.1%

용매

water

반응 조건

후처리

1. 1
   기타the tube was sealed
2. 2
   기타was adjusted to room temperature
3. 3
   추출followed by extraction with ethyl acetate
4. 4
   세척The resultant was washed with saturated saline
5. 5
   건조dried over anhydrous sodium sulfate
6. 6
   workup.DISTILLATIONSubsequently, the solvent was distilled away under reduced pressure
7. 7
   기타the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=50:1 to 4:1)

실험 절차

Dibromomethane (91 mg) and cesium carbonate (380 mg) were added to a tube containing a DMF (4 ml) solution containing 5-bromopyridin-2,3-diol (100 mg) and the tube was sealed, followed by stirring at 100° C.-110° C. for 8 hours. The reaction solution was adjusted to room temperature, and water was added, followed by extraction with ethyl acetate. The resultant was washed with saturated saline and dried over anhydrous sodium sulfate. Subsequently, the solvent was distilled away under reduced pressure, the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=50:1 to 4:1), and a brown solid of 5-bromo-[1,3]dioxolo[4,5-b]pyridine (13.8 mg) was thus obtained.

출처