HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 59803663, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 59803681 | HCID 59803681 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | HCID 59803663 | HCID 59803663 | — |
Reaction Steps
To a solution of {8-[(3,4-dimethoxyphenyl)ethynyl]-7-methyl-2,6-dioxo-1-prop-2-ynyl-1,2,6,7-tetrahydro-3H-purin-3-yl}methyl pivalate (471 mg, 0.98 mmol) in a 4:1 mixture of dry tetrahydrofurane and methanol (20 mL) was added lithium hydroxide monohydrate (127 mg, 1.63 mmol). The mixture was stirred at room temperature for 3 h (TLC-control: dichloromethane/methanol, 9.5:0.5, Rf=0.40 for the product). Subsequently the solvent was removed under reduced pressure, the remaining residue was dissolved in water (30 mL) and acidified with diluted hydrochloric acid. The precipitate was filtered under reduced pressure, washed with water and dried at 70° C., yielding 334 mg (93 yield for the deprotection reaction) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08044061B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-766d73ec614e43dc96e2489c79c878bc |
| Source note | uspto-grants-2011_10 |