3-Pyridyl bromide synthesis
- Product Name:3-Pyridyl bromide
- CAS Number:626-55-1
- Molecular formula:C5H4BrN
- Molecular Weight:158
A method for synthesizing 3-bromopyridine, comprising the steps of:
Add 60 g of pyridine and 100 mL of water to a 500 mL three-necked flask, add 40% HBr (160 g, temperature control of 20-30 ℃ during the process of addition) dropwise with stirri
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626-55-1
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Yield:626-55-1 75%
Reaction Conditions:
with sulfuric acid;bromine at 0 - 130; for 8 h;Time;
Steps:
1-4 Example 1
8.8 g of bromine (50 mmol) was added dropwise to 15 ml (185 mmol) and 95% sulfuric acid at 0 ° C, and reacted at 130 ° C for 8 hours.After the reaction, the mixture was cooled and poured into ice water, and the pH was adjusted to 8 with 6N sodium hydroxide, and 60 ml of petroleum ether was extracted three times.After stratification, several layers were dried over anhydrous sodium sulfate, and the desiccant was filtered, and the organic layer was concentrated, and then distilled with a Vigreux fractionation column.Gas phase analysis of the remaining components, detection conditions: N290ml / min, H2120ml / min,The column temperature was 165 ° C, 4 ul was injected, and the yield was 75%.
References:
CN109748856,2019,A Location in patent:Paragraph 0017-0024
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