4,6-dichloro-5-(4-chlorophenyl)-pyriMidine synthesis
- Product Name:4,6-dichloro-5-(4-chlorophenyl)-pyriMidine
- CAS Number:3974-18-3
- Molecular formula:C10H5Cl3N2
- Molecular Weight:259.52
3979-80-4
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Yield:3974-18-3 89 %
Reaction Conditions:
with trichlorophosphate in N,N-dimethyl-aniline at 130;
Steps:
1.3 Step 3: 4,6-Dichloro-5-(p-chlorophenyl)pyrimidine
5-(p-Chlorophenyl)-4,6-pyrimidinediol (example 1, step 2, 16.80 g, 75.7 mmol) was treated with POCl3 (84.7 mL, 908.4 mmol) followed by careful addition of N,N-dimethylaniline (21.1 mL, 171.1 mmol). The resulting mixture was heated to 130° C. for 3 hours, cooled to rt and then slowly poured onto ice/water with stirring. After all ice melted, the solids were removed by filtration, rinsed with H2O and air-dried. The product was obtained as a tan solid. Yield=17.34 g (67 mmol, 89%). HPLC/MS (ESI) m/z 258.8, 261.0, 263.2 (M++H+). Method 1 retention time=3.20 min.
References:
US2022/396564,2022,A1 Location in patent:Paragraph 0265; 0267
108-90-7
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