HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 86620600, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | Thiosemicarbazide | HCID 2723789 | — |
| Reactant | HCID 66699605 | HCID 66699605 | — |
| Catalyst | Dimethylformamide | HCID 6228 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Propan-2-one--water (1/1) | HCID 18366337 | — |
| Product | HCID 86620600 | HCID 86620600 | — |
Reaction Steps
Add oxalyl chloride (0.660 mg, 5.20 mmol) to a solution of 3-[[4-(4-acetyl-3-hydroxy-2-methyl-phenoxymethyl)-phenyl]-(tetrahydro-pyran-2-yloxy)-methyl]-benzoic acid, 1.00 g, 2.04 mmol) in tetrahydrofuran (0.20M). Add dimethylformamide (5 drops). Add pyridine (0.322 g, 4.08 mmol) and thiosemicarbazide (0.223 g, 2.45 mmol). Stir the reaction overnight. Evaporate solvents. Dissolve brown tar in acetone/water. Extract with CH2Cl2 (3×) and ethyl acetate (3×). Combine organic extracts, dry and concentrate to afford the title compound, which was used without further purification (1.20 g, 2.04 mmol, 99%): MS (m/z): 563 (M−H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07598423B2 |
| Source dataset | uspto-grants-2009_10 |
| ORD ID | ord-20f489b857f1425c9f446c64abc8d677 |
| Source note | uspto-grants-2009_10 |