2-Amino-5-bromo-6-methylpyridine synthesis
- Product Name:2-Amino-5-bromo-6-methylpyridine
- CAS Number:42753-71-9
- Molecular formula:C6H7BrN2
- Molecular Weight:187.04
3430-17-9
42753-71-9
General steps: Example 2 Add 650 g of xylene as solvent to the reactor and heat to 115-120°C. The heating was continued under reflux conditions until the water was completely removed. The solvent was cooled to 70°C under nitrogen protection. Subsequently, 22 g of sodium amide was added and the solution was heated to 118-120 °C. Under reflux condition, 102 g of 2-bromo-3-methylpyridine was slowly added dropwise, and after completion of the dropwise addition, the reaction temperature was maintained at reflux for 1 hour. Upon completion of the reaction, the reaction solution was cooled to 45 °C. The reaction solution was then poured into ice water and the upper organic phase was separated. The xylene was concentrated under atmospheric pressure to 220 g remaining and cooled to 10-15 °C with stirring. After crystallization, 100 g of the target product 2-amino-5-bromo-6-methylpyridine was obtained with 99.3% purity and 90.1% yield.
3430-17-9
454 suppliers
$4.00/5g
42753-71-9
402 suppliers
$6.00/5g
Yield:42753-71-9 90.1%
Reaction Conditions:
with sodium amide in 5,5-dimethyl-1,3-cyclohexadiene at 118 - 120; for 1 h;Inert atmosphere;Time;Concentration;
Steps:
2 Example 2
Example 2
To the reaction tank was charged 650g of xylene as a solvent, heated up to 115 ~ 120 deg. C heated under reflux until complete removal of the water; under nitrogen, the solvent was cooled to 70 deg. C, sodium amide was added 22g, and then the solution was heated to 118 to 120 deg. C, was added dropwise under reflux 102g of 2-bromo-3-methylpyridine, the addition was complete, the reaction maintaining the temperature at reflux 1H; After the reaction, the reaction solution was cooled to 45 deg. C, and then poured into ice water, separation of the upper solvent layer; xylene was concentrated at atmospheric pressure, the remaining 220g, stirring cooling to 10 ~ 15 deg. C, crystallization give the desired product 2- methyl-6-amino-5-bromopyridine 100g, content 99.3%, yield 90.1%.
References:
CN105348181,2016,A Location in patent:Paragraph 0023; 0024; 0025
1824-81-3
483 suppliers
$8.00/25g
42753-71-9
402 suppliers
$6.00/5g
1824-81-3
483 suppliers
$8.00/25g
42753-71-9
402 suppliers
$6.00/5g
91872-10-5
225 suppliers
$5.00/1g
1824-81-3
483 suppliers
$8.00/25g
42753-71-9
402 suppliers
$6.00/5g
91872-10-5
225 suppliers
$5.00/1g
126325-46-0
237 suppliers
$10.00/250mg