تفاعل #427649

معادلة التفاعل

5-bromopyridin-2,3-diol

Dibromomethane

cesium carbonate

DMF

→

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

المردود 13.1%

المذيبات

water

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر