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ChemicalBook CAS DataBase List 2,4-Dichloropyrimidine
3934-20-1

2,4-Dichloropyrimidine synthesis

10synthesis methods
Obtained by chlorination of uracil. Add uracil, phosphorus trichloride, and xylene amine into the reaction pot, heat to 130 ℃, reflux for about 45min, slightly cool, put in crushed ice, that is, the precipitation of purple solid, filtered while hot and not dissolved, washed with ice water, vacuum drying, a kind of purple crude, decolorized with petroleum ether (boiling range of 60-90 ℃), recrystallized, obtained 2,4-dichloropyrimidine.
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Yield:3934-20-1 95%

Reaction Conditions:

with dmap;thionyl chloride;bis(trichloromethyl) carbonate at 65 - 70;

Steps:

1 Example 1

Add 1000 mg of 2,4-dihydroxypyrimidine (8.9 mmol) to a 50 mL reaction flask.50mg DMAP and 4mL SOCl2,A turbid liquid is formed. A solution of 5.28 g (17.8 mmol) of BTC in SOCl 2 (4 mL) was slowly added dropwise.Heating in an oil bath, controlling the reaction temperature between 65 and 70 ° C,Cooling reflux reaction with frozen liquid. After the reaction was completed until the reaction of the starting material was completed, the reaction mixture was cooled, and the solvent was evaporated, and then added to 10 mL of ice water, neutralized with sodium carbonate solution to pH = 8 to 9, and extracted with dichloromethane, and the organic layer was separated.After washing with water, brine, and dried over anhydrous sodium sulfate, the solvent was evaporated (or purified) to give 2,4-dichloropyrimidine in a yield of 95%.

References:

CN110204495,2019,A Location in patent:Paragraph 0019; 0020

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