5-METHYL-2-PHENYL-3H-IMIDAZOLE-4-CARBOXYLIC ACID ETHYL ESTER synthesis
- Product Name:5-METHYL-2-PHENYL-3H-IMIDAZOLE-4-CARBOXYLIC ACID ETHYL ESTER
- CAS Number:77335-93-4
- Molecular formula:C13H14N2O2
- Molecular Weight:230.26
100-46-9
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5408-04-8
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77335-93-4
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Yield:77335-93-4 42%
Reaction Conditions:
in acetonitrile; for 5 h;Reflux;
Steps:
10.2
To a solution of compound 27 (5.20 g, 39.0 mmol) in 60 ml acetonitrile was added benzyl amine (3.85 g, 42.8 mmol) and heated to reflux for 5 hours. After cooled to rt, the precipitate was collected and washed with cold acetonitrile to afford compound 28 (3.2 g, 42% yield).LCMS m/z=231 [M+H]+ LC/MS informationColumn: Xbridge C 18 (3.5pm 4.6x50mm)Flow rate^ 1.8 mL/minUV detection wavelength: 254nm u Mobile phase"- [A] is 0.05% TFA-containing aqueoous solution, and [B] is 0.05% TFA- containing acetonitrile solutionFrom 0 to 1.5 minutes, the percentage of [B] in the mobile phase was gradually increased from 5% to 100%. Thereafter a solution of 100% of [B] was used as the mobile phase.retention time= 1.31 minutes.
References:
WO2012/144661,2012,A1 Location in patent:Page/Page column 84
14369-88-1
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77335-93-4
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77335-93-4
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141-97-9
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77335-93-4
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77335-93-4
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98-88-4
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77335-93-4
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