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ChemicalBook CAS DataBase List 2,4-DICHLOROFURO[3,2-D]PYRIMIDINE
956034-07-4

2,4-DICHLOROFURO[3,2-D]PYRIMIDINE synthesis

5synthesis methods
-

Yield:956034-07-4 87%

Reaction Conditions:

with N,N-dimethyl-aniline;trichlorophosphate at 130; for 2 h;

Steps:

10; vii
To a mixture of lH-furo[3,2-d]pyrimidine-2,4-dione (3.0 g, 0.020 mol) in NJf- dimethylaniline (2.0 mL, 0.016 mol) was added phosphorous oxychloride (18.0 mL, 0.193 mol) and the resulting mixture heated at 130 °C for 2 h. The resulting black solution was cooled to RT, then carefully quenched with crushed ice and H2O, then extracted with EtOAc.The organic layer was isolated, dried (MgSO4) and concentrated in vacuo to give the title compound as a tan solid (3.26 g, 87 %). 1H NMR (400 MHz, CDCl3): δ 7.02 (d, J = 2.2 Hz, 1 H) and 8.08 (d, J = 2.2 Hz, 1 H).

References:

F.HOFFMANN-LA ROCHE AG WO2008/152394, 2008, A1 Location in patent:Page/Page column 25; 35

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