HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-Hydroxyphthalimide → 4-Chloro-7-[2-c-methyl-3,5-bis-o-(2,4-dichlorophenylmethyl)-beta-d-ribofuranosyl]-5-(2-phthalimidooxyethyl)-7h-pyrrolo[2,3-d]pyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-Hydroxyphthalimide | HCID 10665 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Diethyl azodicarboxylate | HCID 5462977 | — |
| Reactant | 4-Chloro-7-[2-c-methyl-3,5-bis-o-(2,4-dichlorophenylmethyl)-beta-d-ribofuranosyl]-5-(2-hydroxyethyl)-7h-pyrrolo[2,3-d]pyrimidine | HCID 87505707 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-Chloro-7-[2-c-methyl-3,5-bis-o-(2,4-dichlorophenylmethyl)-beta-d-ribofuranosyl]-5-(2-phthalimidooxyethyl)-7h-pyrrolo[2,3-d]pyrimidine | HCID 87505905 | 85% |
Reaction Steps
To a solution of the compound 2.6 (359.0 mg, 0.54 mmol) in THF (10 mL) were added triphenylphosphine (215.0 mg, 0.82 mmol) and N-hydroxyphthalimide (132.0 mg, 0.0.81 mmol) followed by diethylazodicarboxylate (DEAD) (153 μL, 0.88 mmol), and the solution was stirred overnight at room temperature. The reaction mixture was diluted by adding 10 mL of CH2Cl2 and 10 mL of water. The aqueous layer was extracted three times with CH2Cl2, dried over Na2SO4, filtered and evaporated. The product was purified by flash column chromatography using 15-20% EtOAc in hexanes as eluent gave the desired compound 2.7 (369 mg, 85%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07713941B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-d391a76cd3574d6faf443ead9ea6137e |
| Source note | uspto-grants-2010_05 |