4(3H)-Quinazolinone,3-methyl-6-nitro- synthesis
- Product Name:4(3H)-Quinazolinone,3-methyl-6-nitro-
- CAS Number:16064-13-4
- Molecular formula:C9H7N3O3
- Molecular Weight:205.17
6943-17-5
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Yield:16064-13-4 83.85%
Reaction Conditions:
with Cs2CO3 in N,N-dimethyl-formamide at 0 - 20; for 3 h;Inert atmosphere;
Steps:
428.1 Step 1: 3-methyl-6-nitroquinazolin-4-one
Into a 250 mL round-bottom flask were added 6-nitro-3H-quinazolin-4-one (10.0 g,52.31 mmol)and Cs 2CO 3 (25.57 g,78.44 mmol)in dimethylformamide (150 mL)at room temperature. CH 3I (11.14 g,78.45 mmol) was added in portions at 0 under nitrogen atmosphere. The resulting mixture was stirred for 3 h at room temperature under nitrogen atmosphere. The resulting mixture was extracted with EtOAc (350 mL) . The combined organic layers were washed with brine (100 mL) , dried over anhydrous Na 2SO 4. After filtration, the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography, eluted with PE/EtOAc (1: 1) to afford the product (9 g, 83.85%) . [M+H] + = 206.2.
References:
WO2022/12622,2022,A1 Location in patent:Page/Page column 323-324
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