3-METHYLQUINAZOLINE-2,4(1H,3H)-DIONE synthesis
- Product Name:3-METHYLQUINAZOLINE-2,4(1H,3H)-DIONE
- CAS Number:607-19-2
- Molecular formula:C9H8N2O2
- Molecular Weight:176.17
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607-19-2
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Yield:607-19-2 90%
Reaction Conditions:
in N,N-dimethyl-formamide at 135 - 145;
Steps:
3-Methyl- 1 H-quinazoline-2,4-dione
solution of 2-amino-N-methylbenzamide (15 g, 0.10 mol) and 1 ,1 - carbonyldiimidazole (21 g, 0.13 mol) in N,N-dimethylformamide (150 mL) was heated at 135-145 °C overnight. The reaction showed 30% starting material by LC so more 1 ,1 - carbonyldiimidazole (14 g, 0.086 mol) was added and the reaction mixture was heated at 140 °C overnight. The reaction showed complete conversion so was cooled and poured into ice/water (300 mL) and stirred for 10 min. The suspension was filtered and the product was washed with water. The solid was dried in the vacuum oven at 50 °C overnight to give 3-methylquinazoline-2,4(1 H,3H)-dione (15.8 g, 0.090 mol, 90%). 1H NMR (300MHz, DMSO-d6) δ = 1 1 .44 (br. s, 1 H), 7.93 (dd, J = 1 .5, 7.8 Hz, 1 H), 7.65 (app. t, J = 7.7 Hz, 1 H), 7.23 - 7.15 (m, 2H), 3.33 (s, 3H)
References:
WO2016/92326,2016,A1 Location in patent:Paragraph 00197; 00198
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607-19-2
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607-19-2
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607-19-2
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$175.00/500mg