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ChemicalBook CAS DataBase List 2,5-Dibromopyrimidine

2,5-Dibromopyrimidine synthesis

5synthesis methods
-

Yield:32779-37-6 73.2%

Reaction Conditions:

Stage #1: 5-bromo-2-aminopyrimidinewith hydrogen bromide;bromine in water at 0 - 4;Inert atmosphere;
Stage #2: with sodium nitrite in water at 0 - 4; for 3 h;

Steps:

2 Example 2

Under nitrogen protection, 34.8 g (0.2 mol) of 2-amino-5-bromopyrimidine and 180 mL of 48% HBr aqueous solution were put into the reaction flask, and 48.0 g (0.3 mol) of bromine was added at 0-4°C to form a yellow suspension. 55.2 g (0.4 mol) of a 50% aqueous solution of sodium nitrite was added dropwise at a temperature of 0-4 °C. After the addition, the mixture was stirred at 0-4° C. for 3 h, the raw material was less than 3% detected by HPLC, and then poured into 100 mL of ice. Neutralize with 30% aqueous sodium hydroxide solution and adjust pH=10-11, and extract with dichloromethane, the organic phase is concentrated to no flow, and then recrystallized with 100 mL ethyl acetate: petroleum ether=1:4 to obtain a white solid 2,5-dibromopyrimidine 34.83 g, yield 73.2%,

References:

CN113683571,2021,A Location in patent:Paragraph 0031-0033

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