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ChemicalBook CAS DataBase List 4,6-DICHLORO-2-(METHYLTHIO)PYRIMIDINE-5-CARBONITRILE
33097-13-1

4,6-DICHLORO-2-(METHYLTHIO)PYRIMIDINE-5-CARBONITRILE synthesis

3synthesis methods
-

Yield: 93%

Reaction Conditions:

with thionyl chloride at 20 - 75; for 3 h;

Steps:

57.57a
To 4,6-dichloro-2-(methylthio)-5-pyrimidinecarbaldehyde oxime (2.38 g, 10 mmol) was added SOCl2 (21.8 mL, 0.30 mol) slowly at room temperature. The solution was then heated at 75 0C for about 3 hours before it was concentrated under vacuum. The residue SOCl2 was removed by evaporation with toluene (5 mL) under vacuum. The resulting solid was washed with EtOH/H2O (1OmL, 1 : 1) to afford 4,6-dichloro-2-(methylthio)-5-pyrimidinecarbonitrile (2.04 g, 93%). LC-MS m/z 220 (M + H)+1.99 minute; 1H-NMR (CDCl3) δ 2.64(3 H).

References:

GLAXO GROUP LIMITED WO2006/104917, 2006, A2 Location in patent:Page/Page column 81-82

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