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ChemicalBook CAS DataBase List 2,4-DIBROMOPYRIMIDINE
3921-01-5

2,4-DIBROMOPYRIMIDINE synthesis

3synthesis methods
Uracil

66-22-8

2,4-DIBROMOPYRIMIDINE

3921-01-5

The general procedure for the synthesis of 2,4-dibromopyrimidine from pyrimidine-2,4(1H,3H)-dione was as follows: phosphorus bromide (40.13 g, 0.14 mol) was mixed with uracil (3 g, 0.027 mol) and the reaction was stirred for 2 hr at 125 °C. After completion of the reaction, it was cooled to room temperature and the reaction mixture was slowly poured into 500 g of ice water and neutralized with solid sodium bicarbonate. Subsequently, the aqueous phase was extracted twice with 150 ml of dichloromethane. The organic phases were combined, dried and concentrated under reduced pressure to give 6.2 g of crude product. Finally, the crude product was purified by fast silica gel column chromatography to give 5 g of white solid product in 78.5% yield.

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Yield: 78.5%

Reaction Conditions:

with phosphorus(V) oxybromide at 125; for 2 h;Temperature;Concentration;

Steps:

1.1 Example 1 The first step: 2,4-dibromopyrimidine synthesis
A mixture of phosphorus oxybromide (40.13 g, 0.14 mol) and uracil (3 g, 0.027 mol) was stirred at 125 ° C for 2 hours. The reaction was allowed to cool to room temperature and the reaction mixture was slowly poured into 500 g of ice water and washed with solid sodium bicarbonate Neutralization reaction. The aqueous phase is extracted twice with 150 ml of methylene chloride. The organic phase was dried and dried under reduced pressure to give 6.2 g of crude product,The crude product was then purified on a flash silica gel column to give 5 g of a white solid (yield: 78.5%).

References:

Shanghai Zaiqi Biological Co., Ltd.;Wang Zhiguo;Song Yanhong;Ma Xiujuan;Tian Beibei;Li Shijiang;Li Chao;Li Qiang;Li Tao CN106632077, 2017, A Location in patent:Paragraph 0017; 0018; 0019; 0025; 0026; 0027; 0032-0034

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