Pyrimidine, 4,5-dichloro-2-(methylthio)- synthesis
- Product Name:Pyrimidine, 4,5-dichloro-2-(methylthio)-
- CAS Number:99469-85-9
- Molecular formula:C5H4Cl2N2S
- Molecular Weight:195.07
61044-94-8
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$57.00/25mg
99469-85-9
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Yield: 86%
Reaction Conditions:
Stage #1:5-chloro-2-methylthio-4(1H)-pyrimidinone with trichlorophosphate for 2 h;Reflux;
Stage #2: with water;potassium carbonate; pH=7 - 8
Steps:
3
A suspension of 5-chloro-2-(methylthio)pyrimidin-4(3H)-one (24 g, 0.136 mol) in POCI3 (200 mL) was heated at reflux for 2 hrs. The reaction mixture was then cooled to room temperature and was concentrated to remove excessive of POCI3. The residue was then treated with H2O (150 mL) and was adjusted to pH=7~8 with aq. K2CO3. The resulting mixture was extracted with CH2CI2 (50 mL χ 4). The combined organic layers were washed with brine (50 mL), dried over Na2SO4 and filtered. The filtrate was concentrated and dried on vacuum to give title compound (23 g, 86%) as a light brown solid.
References:
PFIZER INC.;NAIR, Sajiv, Krishnan;PLANKEN, Simon, Paul WO2012/52948, 2012, A1 Location in patent:Page/Page column 53
5751-20-2
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99469-85-9
66 suppliers
$25.00/250mg