ChemicalBook CAS DataBase List 4,8-dichloropyrido[3,4-d]pyriMidine

4,8-dichloropyrido[3,4-d]pyriMidine synthesis

5synthesis methods

Product Name:4,8-dichloropyrido[3,4-d]pyriMidine
CAS Number:1260663-37-3
Molecular formula:C7H3Cl2N3
Molecular Weight:200.02

84341-13-9 Synthesis

8-chloro-3H-pyrido[3,4-d]pyrimidin-4-one

84341-13-9
29 suppliers
$101.00/50mg

1260663-37-3
31 suppliers
$45.00/2.5mg

Yield:1260663-37-3 11%

Reaction Conditions:

with N-ethyl-N,N-diisopropylamine;trichlorophosphate at 0 - 110; for 2 h;

Steps:

4,8-dichloropyrido[3,4-d]pyrimidine:

DIPEA (426.5 mg, 3.3 mmol) was added dropwise to a mixture of 8-chloropyrido[3,4-d]pyrimidin-4(3H)-one (400 mg, 2.20 mmol) in POCI3(13.20 g, 86.1 mmol) at 0°C and the mixture was stirred at 110°C for 2 h. The solvent was removed and water (15 mL) was added slowly and adjusted to pH 8 with sat. aq. NaHCCE and the mixture extracted with EtOAc (2 x 30 mL). The combined organics were washed with brine (30 mL), dried (NaiSO and evaporated to dryness in vacuo. The residue was purified by silica gel column (petroleum ether/EtOAc; 3: 1 to 0: 1) to give the title compound as a white solid (50 mg, 11%). 1H NMR (500 MHz, DMSO-d6) d: 9.38 (br s, 1H), 8.70 (d, 7=5.5 Hz, 1H), 8.17 (d, 7=6.0 Hz, 1H).

References:

WO2020/163193,2020,A1 Location in patent:Paragraph 00248

58483-94-6 Synthesis