HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Nitrobenzoic Acid → HCID 178525747, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Nitrobenzoic Acid | HCID 6108 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| Reactant | HCID 178515017 | HCID 178515017 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178525747 | HCID 178525747 | — |
Reaction Steps
To a solution of trans-2-(4-Hydroxy-cyclohexyl)-isoindole-1,3-dione (38 g, 154.9 mmol), triphenylphosphine (65 g, 248 mmol), and 4-nitrobenzoic acid (41.4 g, 248 mmol) in 1500 mL of THF was added dropwise diisopropyl azodicarboxylate (50.1 g, 248 mmol) at room temperature. The reaction mixture was stirred overnight. The solvent was evaporated, and the resulting solid was recrystallized from methanol. Yield: 53 g (86.7% of theory). 1H NMR (300 MHz, CDCl3): δ 8.40-8.36 (m, 4H), 7.79 (ddd, J=0.12, 0.02, and 0.02 Hz, 4H), 5.39 (s, 1H), 4.37-4.22 (m, 1H), 2.82-2.65 (m, 2H), 2.27-2.16 (m, 2H), 1.84-1.65 (m, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08476043B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-b4e8ea132ff34972b55e36f4b0764218 |
| Source note | uspto-grants-2013_07 |