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7-CHLOROPYRIDO[3,2-D]PYRIMIDIN-4(3H)-ONE synthesis

3synthesis methods
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Yield:897360-16-6 1.03 g

Reaction Conditions:

at 155; for 22 h;

Steps:

11.2 7-Chloropyrido[3,2-d]pyrimidin-4(1H)-one

A suspension of 3-amino-5-chloropicolinamide (1.1 g, 6.41 mmol) in triethyl orthoformate (15.99 mL, 96 mmol) was stirred at 155° C. for 22 hours. After cooling to RT, the yellow precipitate was collected by vacuum filtration and washed with hexanes to yield the title intermediate (1.03 g, 5.67 mmol) as a yellow solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 8.20 (s, 1H) 8.27 (d, J=2.35 Hz, 1H) 8.80 (d, J=2.25 Hz, 1H) 12.68 (br. s., 1H). LC/MS (ESI m/z=182 (M+H).

References:

US2014/213581,2014,A1 Location in patent:Paragraph 0628

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