HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 18173123, compound → HCID 18173107, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 18173123 | HCID 18173123 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Catalyst | Methyltriphenyliphosphonium bromide | HCID 74505 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18173107 | HCID 18173107 | — |
Reaction Steps
Methyl-triphenyl-phosphonium bromide (2.08 g) was taken in THF (50 ml) at −78° C. nBuLi (3.66 ml, 1.6 M) was added slowly at −78° C. and stirred for 1 hr. 8-(5-Oxo-tricyclo[2.2.1.02,6]hept-3-yl)-1,3-dipropyl-3,7-dihydro-purine-2,6-dione (Example 1) (1 g) was dissolved in THF and added to the reaction mixture at −78° C. slowly. After the addition was over, the reaction mixture was allowed to warmed to room temperature slowly and stirred at room temperature overnight. The next day, the reaction mixture was quenched with 1N HCl and extracted with ethyl acetate (3×50 ml). The combined organic layer was washed with water, brine and dried over Na2SO4. After concentration the product was purified by silica gel column. Mass (ES+ 341).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06605600B1 |
| Source dataset | uspto-grants-2003_08 |
| ORD ID | ord-39217ac792cd4e2a85e58a7eaff5a94e |
| Source note | uspto-grants-2003_08 |