Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 178462983 | HCID 178462983 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18549213 | HCID 18549213 | 94.2% |
Reaction Steps
Next, potassium carbonate (8.15 g, 59.0 mmol) was added to DMF (100 ml) solution of 3-ethyl-2-mercapto-6-trifluoromethyl-4(3H)-pyrimidinone (11.0 g, 49.0 mmol), methyl iodide (3.68 ml, 59.0 mmol) was added with stirring under ice-cooling, followed by stirring for 4 hours while gradually returning to room temperature. After completion of the reaction, the reaction solution was concentrated under a reduced pressure, water (100 ml) and ethyl acetate (100 ml) were added to the thus obtained residue to separate the organic layer, and then the aqueous layer was extracted with ethyl acetate (50 ml×3). The organic layers were combined, washed with water (100 ml×3) and saturated brine (300 ml) and then dried over anhydrous magnesium sulfate. The drying agent was removed by filtration and then the resulting filtrate was concentrated under a reduced pressure to obtain 3-ethyl-2-methylthio-6-trifluoromethyl-4(3H)-pyrimidinone (11.0 g, 94%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06548511B1 |
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| Source dataset | uspto-grants-2003_04 |
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| ORD ID | ord-a048c0b4e8b64bc49aa20e6196be5539 |
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| Source note | uspto-grants-2003_04 |
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