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ChemicalBook CAS DataBase List 5-Bromo-4-chloro-2,6-dimethylpyrimidine
69696-35-1

5-Bromo-4-chloro-2,6-dimethylpyrimidine synthesis

4synthesis methods
5-broMo-2,6-diMethylpyriMidin-4-ol

858269-28-0

5-Bromo-4-chloro-2,6-dimethylpyrimidine

69696-35-1

(b) Synthesis of 5-bromo-4-chloro-2,6-dimethylpyrimidine. 5-Bromo-2,6-dimethylpyrimidin-4-ol (3.95 g, 19.45 mmol) was mixed with phosphorochloridic acid (6 mL, 64.4 mmol) and heated to reflux for 3 h at 110 °C. The reaction was carried out at a pressure of 1.5 °F. Upon completion of the reaction, the reaction solution was concentrated under reduced pressure, followed by the slow and careful addition of ice water to precipitate a white precipitate. The solid was collected by filtration, washed thoroughly with cold water and dried to afford the target product 5-bromo-4-chloro-2,6-dimethylpyrimidine (2.73 g, 63% yield). The product was analyzed by LCMS (ES+), m/e 221 [M+H]+.

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Yield:69696-35-1 63%

Reaction Conditions:

with trichlorophosphate at 110; for 3 h;

Steps:

56.b b) 5-bromo-4-chloro-2,6-dimethylpyrimidine

b) 5-bromo-4-chloro-2,6-dimethylpyrimidine. A mixture of 5-bromo-2,6- dimethylpyrimidin-4-ol (3.95 g, 19.45 mmol) and phosphorus oxychloride (6 mL, 64.4 mmol) was heated at 1 10 °C for 3h. The solution was concentrated, and water was then added slowly and cautiously to afford a precipitate. The solid was filtered and washed with water, and dried to give the title compound (2.73 g, 63%). LCMS (ES+) m/e 221 [M+H]+.

References:

WO2013/96151,2013,A1 Location in patent:Page/Page column 131

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