Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | 2-(Methylthio)-1H-pyrimidin-4-one | HCID 79823 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | AC1NR783 | HCID 5235666 | 48.5% |
Reaction Steps
To a mixture of HOAc (500 mL) and Ac2O (10 mL) was added compound 2-(methylthio)pyrimidin-4(3H)-one (40 g, 0.28 mol). The resulting mixture was heated at 80° C. for 30 min to remove any moisture. Then NCS (49 g, 0.37 mol) was added at 50˜60° C. The resulting mixture was stirred at 50˜60° C. for 24 h. The mixture was then cooled to room temperature and was poured into ice-water (500 mL). The solid formed was collected and was treated with MeOH (100 mL) at reflux. Then the solid was filtered and dried on vacuum to give title compound (24 g, 48%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09056865B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-45469990c9eb495d9b1786a61e7f73e9 |
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| Source note | uspto-grants-2015_06 |
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