반응 #163278

반응 방정식

potassium bromate

potassium bromate

3,5-dimethoxypyridine

hydrochloric acid

potassium bromide

sulfuric acid

sodium sulfite

potassium bromide

→

2,6-dibromo-3,5-dimethoxypyridine

수율 83.9%

용매

water

pyridine

water

water

반응 조건

후처리

1. 1
   workup.STIRRINGThe reaction was stirred for ten minutes
2. 2
   기타The solid was collected by Buchner funnel
3. 3
   세척washed with water
4. 4
   workup.DISSOLUTIONdissolved in dichloromethane
5. 5
   건조dried over sodium sulfate
6. 6
   기타evaporated

실험 절차

A flask was charged with 3,5-dimethoxypyridine (13 g; 93 mmol), water (100 mL) and concentrated hydrochloric acid (8 mL; ˜1 eq.). To a separate flask was added potassium bromide (65 g.), water (200 mL) and sulfuric acid (69 g.). To a third flask was added potassium bromate (18 g.), and water (1.2 liters). All flasks were stirred until they were homogenous. To the flask with potassium bromate was added the solution containing potassium bromide, followed by the solution containing the pyridine compound. The reaction was stirred for ten minutes, and a solution of sodium sulfite was added until the orange color disappeared. The solid was collected by Buchner funnel, washed with water, dissolved in dichloromethane, dried over sodium sulfate, and evaporated to give 2,6-dibromo-3,5-dimethoxypyridine (23.3 g; 78 mmol).

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