ChemicalBook CAS DataBase List 2,6-Dichloro-4,8-dipiperidinopyrimidino[5,4-d]pyrimidine

2,6-Dichloro-4,8-dipiperidinopyrimidino[5,4-d]pyrimidine synthesis

7synthesis methods

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

2,4,6,8-TETRACHLOROPYRIMIDO[5,4-D]PYRIMIDINE

32980-71-5

2,6-Dichloro-4,8-dipiperidinopyrimidino[5,4-d]pyrimidine

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
0 suppliers
$15.96/100ML

32980-71-5
122 suppliers
$137.00/1G

7139-02-8
117 suppliers
$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 Synthesis