Pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione, 1-methyl- synthesis
- Product Name:Pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione, 1-methyl-
- CAS Number:142168-85-2
- Molecular formula:C8H7N3O2
- Molecular Weight:177.16
Yield:142168-85-2 17%
Reaction Conditions:
in toluene at 110; for 12 h;
Steps:
84.3 1-Methylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione
2-(Methylamino)pyridine-3-carboxamide (100 mg, 0.661 mmol) and phenylisocyanate (157 mg, 1.32 mmol) were dissolved in toluene (10 mL) and stirred at 110°C for 12 hours.
The reaction was quenched by adding water (10 mL) and filtered to give 1-methylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione (20.0 mg, as a yellow solid) with a yield of 17%. 1H NMR: (400 MHz, DMSO-d6) δ 11.72(s, 1H), 8.72(d, J = 2.0 Hz, 1H), 8.31(d, J = 7.6 Hz, 1H), 7.29(dd, J = 7.6, 2.0 Hz, 1H), 3.48(s, 3H). MS-ESI calcd. [M + H]+ 178, found 178.
References:
EP3299371,2018,A1 Location in patent:Paragraph 0528; 0531
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