HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phthalimide → HCID 58929738, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phthalimide | HCID 6809 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | 1044942-90-6 | HCID 58929728 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58929738 | HCID 58929738 | — |
Reaction Steps
A solution of diethyl azodicarboxylate (0.56 mL, 3.6 mmol) in anhydrous THF (3.0 mL) was added drop-wise to a mixture of (1R,2R,4R)-5,5-difluorobicyclo[2.2.1]heptan-2-ol (0.44 g, 3.0 mmol), phthalimide (0.50 g, 3.4 mmol), and triphenyl phosphine (0.78 mL, 3.4 mmol) in anhydrous tetrahydrofuran (15.0 mL) at r.t. under nitrogen. After stirring at ambient temperature for 66 h, the solvents were removed in vacuo. The residue was partitioned between ethyl acetate and water, and the organic portion was separated, washed with brine, and conc. in vacuo. Flash column chromatography (0 to 35% of ethyl acetate in hexanes) gave the title compound as an off-white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07253196B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-c00de8275eee46d299b5ea8240cba241 |
| Source note | uspto-grants-2007_08 |