Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Lithium Carbonate | HCID 11125 | — |
| Reactant | (8E)-8-[(2Z)-2-(3-hydroxy-4-oxo-1-cyclohexa-2,5-dienylidene)ethylidene ]-7-methyl-1,3-dipropyl-9H-purine-2,6-dione | HCID 135665338 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 151539-57-0 | HCID 6448807 | 31.3% |
Reaction Steps
Compound 53 (500 mg, 1.30 mmol) obtained in Reference Example 46 was dissolved in 10 ml of dimethylformamide. To the solution were added 0.40 ml (6.43 mmol) of methyl iodide and 400 mg (6.50 mmol) of lithium carbonate, and the mixture was stirred at 80° C. for 5 hours. Water was added thereto to dissolve lithium carbonate and deposited crystals were collected by filtration. The collected crude crystals were dissolved in chloroform, washed with a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate, followed by evaporation under reduced pressure. The residue was purified by silica gel column chromatography (eluent:chloroform) to give 162 mg (yield 31%) of Compound 63 as yellow grains.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05587378 |
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| Source dataset | uspto-grants-1996_12 |
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| ORD ID | ord-c6fda76b73714c22ad154e646971baca |
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| Source note | uspto-grants-1996_12 |
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