2,6-Dichloro-4,8-dipiperidinopyrimidino[5,4-d]pyrimidine synthesis
- Product Name:2,6-Dichloro-4,8-dipiperidinopyrimidino[5,4-d]pyrimidine
- CAS Number:7139-02-8
- Molecular formula:C16H20Cl2N6
- Molecular Weight:367.28
110-89-4
32980-71-5
7139-02-8
General procedure for the synthesis of 2,6-dichloro-4,8-dipiperidinosubstituted pyrimido[5,4-d]pyrimidines from hexahydropyridine and perchloropyrimido[5,4-d]pyrimidines: perchloropyrimido[5,4-d]pyrimidines (13.1 g, 48.9 mmol), piperidines, CuI (0.28 g, 1.5 mmol) and Cs2CO3 (16.0 g, 48.9 mmol) were added to a 250mL two-necked flask. 100 mL of nitrobenzene was added as reaction solvent and the reaction was carried out at 180°C for 16 h under nitrogen protection. After completion of the reaction, the nitrobenzene solvent was removed by distillation under reduced pressure. Purification by column chromatography using a solvent mixture of petroleum ether (PE) and dichloromethane (DCM) (6:1, v/v) gave 17.0 g of solid product in 95.0% yield and 99% selectivity.
110-89-4
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32980-71-5
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7139-02-8
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$6.00/250mg
Yield:7139-02-8 95%
Reaction Conditions:
with copper(l) iodide;caesium carbonate in nitrobenzene at 180; for 16 h;Inert atmosphere;
Steps:
4.g Example 4: Synthesis of perchloropyrimido [5,4-d] pyrimidine
the entire chlorine pyrimido [5, 4 - d] pyrimidine (13.1 g, 48.9 mmol), piperidine, CuI (0.28 g, 1.5 mmol), Cs2 CO3 (16.0 g, 48.9 mmol) is put into the 250 in two mouth flask, add 100 ml nitrobenzene as the reaction solvent, under the protection of nitrogen, 180 °C lower reaction 16 h, oil pump by reducing pressure after the reaction of the nitrobenzene solvent, PE:DCM=6:1 to column chromatography, obtaining the solid 17.0 g, yield of 95.0%, the selectivity 99%
References:
CN106946887,2017,A Location in patent:Paragraph 0035; 0036; 0037
6713-54-8
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7139-02-8
119 suppliers
$6.00/250mg