2,4-Dichloropyrido[3,4-d]pyrimidine synthesis
- Product Name:2,4-Dichloropyrido[3,4-d]pyrimidine
- CAS Number:908240-50-6
- Molecular formula:C7H3Cl2N3
- Molecular Weight:200.02
![PYRIDO[3,4-D]PYRIMIDINE-2,4(1H,3H)-DIONE](/CAS/GIF/21038-67-5.gif)
21038-67-5
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$75.00/100mg
908240-50-6
110 suppliers
$45.00/2.5mg
Yield:908240-50-6 82%
Reaction Conditions:
with N-ethyl-N,N-diisopropylamine;trichlorophosphate in toluene at 25; for 18 h;
Steps:
B; 47.2; 136.2 Step B:
To a mixture of pyrido[3,4-d]pyrimidine-2,4(1 H,3H)-dione (2b, 20.00 g, 122.60 mmol) and POCI3 (328.03 g, 2.14 mol) in toluene (200 mL) was added DIEA (31 .69 g, 245.20 mmol) dropwise and this reaction mixture stirred at 25°C overnight (18hr) to give suspension. The solvent and POCI3 was removed under vacuum, diluted with DCM (50 mL), neutralized with DIEA to pH=7 at -20°C and concentrated again, the residue was purified by column (20-50% EA/PE) to give the product (2c, 20.00g, 99.99 mmol, 82% yield) as a yellow solid. 1 H NMR (400 MHz, CHLOROFORM-d) δ 9.52 (s, 1 H), 8.92 (d, J=5.6 Hz, 1 H), 8.04 (d, J=5.6 Hz, 1 H). LCMS (m/z [M+H]+): 200.0.
References:
NOVARTIS AG;BEHNKE, Dirk;BERENSHTEYN, Frada;HAO, Xueshi;HOFFMAN, Timothy;JIN, Qihui;LACOSTE, Arnaud;LEE, Cameron;LIU, Jun;LIU, Yahu;MAIBAUM, Juergen Klaus;MO, Tingting;PAN, Jianfeng;QU, Xin;TCHORZ, Jan;XIE, Yun Feng;YAN, Shanshan;ZOU, Yefen WO2018/198077, 2018, A2 Location in patent:Page/Page column 189; 197; 225; 226; 262; 263
7579-20-6
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$10.00/1g
908240-50-6
110 suppliers
$45.00/2.5mg
64188-97-2
98 suppliers
$8.00/100mg
908240-50-6
110 suppliers
$45.00/2.5mg