Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Thiazole | HCID 9256 | — |
| Reactant | 4-Fluoroiodobenzene | HCID 9605 | — |
| Reactant | Potassium Acetate | HCID 517044 | — |
| Catalyst | Palladium hydroxide | HCID 9942167 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | 5-(4-Fluorophenyl)thiazole | HCID 21709651 | 22% |
Reaction Steps
To a sealed tube containing a solution of thiazole (2 g, 23.53 mmol) in DMA (10 mL) was added potassium acetate (6.9 g, 70.58 mmol), 1-fluoro-4-iodobenzene (15.6 g, 70.58 mmol), and palladium hydroxide\C (0.53 g, 2.35 mmol) under nitrogen. The reaction mixture was heated to 145° C. and stirred for 16 h. The reaction mixture was cooled to room temperature and diluted with water (200 mL), filtered through Celite® reagent, and extracted with ethyl acetate (300 mL). The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure to obtain crude product. The crude product was purified by column chromatography (100-200μ silica gel, eluting with 10% EtOAc and hexane) to afford 5-(4-fluorophenyl)thiazole (0.9 g, 22%). 1H NMR (400 MHz, CDCl3): δ 8.74 (s, 1H), 8.01 (s, 1H), 7.55 (t, 2H), 7.11 (t, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08809372B2 |
|---|
| Source dataset | uspto-grants-2014_08 |
|---|
| ORD ID | ord-2776c3d228b44ba38b2fe6c201cfca11 |
|---|
| Source note | uspto-grants-2014_08 |
|---|