4-Bromo-2-methylpyridine synthesis

11synthesis methods

Product Name:4-Bromo-2-methylpyridine
CAS Number:22282-99-1
Molecular formula:C6H6BrN
Molecular Weight:172.02

18437-58-6
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22282-99-1
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$6.00/5g

Yield:22282-99-1 95%

Reaction Conditions:

with hydrogen bromide;bromine at -5;

Steps:

1.3 (3) Preparation of 2-methyl-4-bromopyridine:
2-Methyl-4-aminopyridine (10.8 g, 0.1 mol) was added to 48% HBr (46 ml, 0.4 mol) with ice-cooling.After the addition is completed, the mixture is cooled to -5 ° C, and liquid bromine (15 ml, 0.3 mol) is slowly added dropwise, and the addition is completed in 30-35 minutes.Then, 42% of a 40% sodium nitrite solution was added dropwise at 0 ° C or less, and the addition was completed in 1-1.1 h.After the addition is completed, the mixture is stirred at 0 ° C for 30 min, and then slowly added with 50% sodium hydroxide solution below 20 ° C to adjust the pH of the solution to 9,The reaction solution was extracted with ethyl acetate, dried over anhydrous sodium sulfate grassroots, suction filtered, and concentrated2-Methyl-4-bromopyridine was obtained in a molar yield of 95%.

References:

Danyang Ning David Fang To Detect Co., Ltd.;Wei Qian CN109748854, 2019, A Location in patent:Paragraph 0018; 0021

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