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ChemicalBook CAS DataBase List 2,4-Dichloro-6-methyl-5-nitropyrimidine

2,4-Dichloro-6-methyl-5-nitropyrimidine synthesis

5synthesis methods
-

Yield:13162-26-0 65%

Reaction Conditions:

with N,N-dimethyl-aniline;trichlorophosphate in N,N-dimethyl-formamide at 120; for 8 h;

Steps:

15 Example 15: Synthesis of Compound 13

The raw material 12 (1 eq) was dissolved in 17.54 ml of phosphorus oxychloride, and 2.92 ml of N, N-dimethylaniline (1 eq) was slowly added dropwise at room temperature, and 8.04 ul of DMF (0.00445 eq) 120 under reflux reaction 8h, after the completion of the reaction of raw materials, vacuum distillation of phosphorus oxychloride, adding ice water, adding ethyl acetate extraction, combined organic layer, washed with saturated brine, dried over anhydrous sodium sulfate, spin dry Solvent to give a yellowish brown oil which was dryly chromatographed and finally purified to give a yellow solid 13 (1 g) in 65% yield.

References:

CN105906621,2016,A Location in patent:Paragraph 0031

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