Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 5-Iodo-2,4-dimethoxypyrimidine | HCID 263416 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 59326879 | HCID 59326879 | — |
Reaction Steps
2,4-Dimethoxy-5-iodopyrimidine Z (2.54 g, 9.6 mmol) was added to 26 ml of 5N sodium hydroxide in 50% aqueous methanol and the resulting solution was refluxed overnight. The reaction mixture was evaporated to dryness under reduced pressure, diluted to 25 ml with water and neutralized to ph ˜6 with 1N hydrochloric acid. The precipitate was filtered off, washed with water (2×10 ml), methanol (2×10 ml) and diethyl ether to give 0.55 g of pure product. The filtrate was concentrated under reduced pressure and kept overnight at 4° C. The crystals of the product were filtered off washed as above to give additional 0.3 g of pure product as a colorless crystals (total yield 0.85 g, 35%). 1HNMR (DMSO-d6, 300 MHz) δ 8.14 (s, 1H) 3.82 (s, 3H); 3.3 (broad s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08466163B2 |
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| Source dataset | uspto-grants-2013_06 |
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| ORD ID | ord-c7e6dcdc53594075bea28e5f80c7ff70 |
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| Source note | uspto-grants-2013_06 |
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