ChemicalBook CAS DataBase List 4,6-DICHLORO-5-ETHYLPYRIMIDINE

4,6-DICHLORO-5-ETHYLPYRIMIDINE synthesis

4synthesis methods

Product Name:4,6-DICHLORO-5-ETHYLPYRIMIDINE
CAS Number:53967-81-0
Molecular formula:C6H6Cl2N2
Molecular Weight:177.03

4(1H)-Pyrimidinone, 5-ethyl-6-hydroxy- (9CI)

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Yield:53967-81-0 95%

Reaction Conditions:

Stage #1: 5-ethylpyrimidine-4,6-diolwith trichlorophosphate for 1 h;Heating / reflux;
Stage #2: with N,N-diethylaniline at 20; for 4 h;Heating / reflux;

Steps:

1

A mixture of 5 g (35.7 mmoles) of 5-ethyl-4,6-dihydroxy-pyrimidine (marketed by Aldrich) in 30 ml of phosphorus oxychloride is taken to reflux for 1 hour. After returning to ambient temperature, a mixture of 4 ml of N,N-diethylaniline in 10 ml of phosphorus oxychloride is added dropwise and the reaction medium is taken to reflux for 4 hours. After returning to ambient temperature, the reaction medium is poured into a mixture of ice and water, followed by extracting with ethyl acetate, washing the organic phases with 2N hydrochloric acid, drying over magnesium sulphate and evaporating to dryness under vacuum. 6 g (Yield=95%) of a brown oil of expected product is obtained used as it is for the following. TLC: Rf=0.5 (silicagel, eluent: dichloromethane-methanol 90-10)

References:

US2006/52398,2006,A1 Location in patent:Page/Page column 11