1-(2-methoxy-4-nitrophenyl)-3-methyl-1H-1,2,4-triazole synthesis
- Product Name:1-(2-methoxy-4-nitrophenyl)-3-methyl-1H-1,2,4-triazole
- CAS Number:1185019-82-2
- Molecular formula:C10H10N4O3
- Molecular Weight:234.21
454-16-0
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7170-01-6
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1185019-82-2
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1232038-78-6
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Yield:1185019-82-2 49% ，1232038-78-6 13%
Reaction Conditions:
with potassium carbonate in dimethyl sulfoxide at 120; for 1 h;
Steps:
A.6.a
A mixture of l-fluoro-2-methoxy-4-nitrobenzene (821.414 mg, 4.8 mmol), 5-methyl- lH-l,2,4-triazole (800 mg, 9.63 mmol), K2CO3 (4.8 mmol) and DMSO (8 ml) was stirred at 120 0C for 1 h. After cooling to r.t., the r.m. was poured into ice H2O. The solid was filtered off, washed with H2O and dried in vacuo at 50 0C. Yield: 0.554 g of intermediate 9 (49 %). The aq. layer was sat. with NaCl, extracted with DCM and the organic layer was dried (MgSO4), filtered and the solvent was evaporated in vacuo. The residue was purified by column chromatography over silicagel (eluent: DCM). The desired fraction was collected and the solvent was evaporated in vacuo. Yield: 0.147 g of intermediate 10 (13 %).
References:
WO2010/70008,2010,A1 Location in patent:Page/Page column 48
7170-01-6
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1009-36-5
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1185019-82-2
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