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CAS No. : | 69696-35-1 | MDL No. : | MFCD13705450 |
Formula : | C6H6BrClN2 | Boiling Point : | 264.9±35.0°C at 760 mmHg |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 221.48 | Pubchem ID : | 12490576 |
Synonyms : |
|
TPSA :Topological Polar Surface Area | 25.8 | H-Bond Acceptor Count : | 2 |
XLogP3 : | 2.7 | H-Bond Donor Count : | 0 |
SP3 : | 0.33 | Rotatable Bond Count : | 0 |
Signal Word: | Warning | Class | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
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Yield | Reaction Conditions | Operation in experiment |
---|---|---|
63% | at 110℃; for 3.00 h; | 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, 63percent). LCMS (ES+) m/e 221 [M+H]+. |
48% | at 110℃; for 18.00 h; | 5-Bromo-4-chloro-2,6-dimethylpyrimidine (B1.2) (0348) A mixture of B1.1 (134 g, 0.66 mol) in 500 mL of POCl3 was stirred at 110° C. for 18 h. Excess POCl3 was removed under vacuum, the residue was poured into 1000 g crushed ice. Then solid NaHCO3 was added carefully to adjust pH to 8-9. The aqueous was extracted with ethyl acetate (1.5 L×3), and the combined organic layers were washed with brine (1.0 L×2), dried over Na2SO4, concentrated to give the title compound (71 g, 48percent) as a white solid. LC-MS: [M+H]+=223.0. |
48% | at 110℃; for 18.00 h; | A mixture of B16.2 (134 g, 0.66 mol) in 500 mL of POCl3 was stirred at 110 C for 18 h. Excess POCl3 was removed under vacuum, the residue was poured into 1000 g crushed ice. Then solid NaHCO3 was added carefully to adjust pH to 8-9. The aqueous was extracted with ethyl acetate (1.5 L × 3), and the combined organic layers were washed with brine (1.0 L × 2), dried over Na2SO4, concentrated to give the title compound (71 g, 48percent) as a white solid. LC-MS: [MH]+ = 223. |
48% | at 110℃; for 18.00 h; | A mixture of BI .1(134 g,0.66 mol) in 500 mL of POd3 was stirred at 110 °C for 18 h. Excess POd3 wasremoved under vacuum, the residue was poured into 1000 g crushed ice. Then solid NaHCO3 was added carefully to adjust pH to 8-9. The aqueous was extracted with ethyl acetate (1 .5 L x 3), and the combined organic layers were washed with brine (1 .0 L x 2), dried over Na2SO4, concentrated to give the title compound (71 g, 48percent) as a white solid. LC-MS: [M+H] = 223.0. |
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