Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Silanamine, 1,1,1-trimethyl-N-(trimethylsilyl)-, potassium salt | HCID 45051783 | — |
| Reactant | HCID 58128634 | HCID 58128634 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58128708 | HCID 58128708 | 66.5% |
Reaction Steps
4-(4-Fluoro-phenyl)-1-methyl-2-oxo-1,2,3,4-tetrahydro-pyrimidine-5-carboxylic acid ethyl ester (1.0 g, 3.6 mmol) was dissolved in 10 mL DMF and cooled to 0°. Potassium hexamethyldisilazane (8 mL, 4 mmol of 0.5M toluene solution) was added and the reaction mixture was stirred at 0° for 5 minutes. CH3I (0.3 mL, 4.8 mmol) was added and the mixture was allowed to warm to room temperature and stir for 2 hours. The solution was poured into cold aqueous pH 2 buffer and extracted with ethyl acetate. The organic layer was dried over Na2SO4, filtered and the solvent removed in vacuo. The residue was chromatographed in 0-30% ethyl acetate/hexane to yield 700 mg of 4-(4-fluoro-phenyl)-1,3-dimethyl-2-oxo-1,2,3,4-tetrahydro-pyrimidine-5-carboxylic acid ethyl ester.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08435990B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-209c71cf0df44c8dbe61f9b51c69035c |
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| Source note | uspto-grants-2013_05 |
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