HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 1H-Purine-2,6-dione,8-[2-(3,4-dihydroxyphenyl)ethenyl]-1,3-diethyl-3,7-dihydro-7-methyl-, (E)-(9CI)
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | Istradefylline | HCID 5311037 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1H-Purine-2,6-dione,8-[2-(3,4-dihydroxyphenyl)ethenyl]-1,3-diethyl-3,7-dihydro-7-methyl-, (E)-(9CI) | HCID 135770338 | 35% |
Reaction Steps
Compound 65 (2.00 g, 5.20 mmol) obtained in Example 8 was dissolved in 40 ml of methylene chloride. To the solution was added 26 ml (26 mmol) of boron tribromide (1.0M methylene chloride solution) under ice cooling in argon atmosphere, and the mixture was stirred overnight at room temperature. Methanol was added thereto and the mixture was separated with chloroform-an aqueous solution of sodium bicarbonate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate, followed by evaporation under reduced pressure. The residue was recrystallized from ethanol to give 643 mg (yield 35%) of Compound 173 as pale yellow grains.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05484920 |
| Source dataset | uspto-grants-1996_01 |
| ORD ID | ord-2784b14369c944d4be2a4d01f543a221 |
| Source note | uspto-grants-1996_01 |