Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formamide | HCID 713 | — |
| Reactant | 4-Bromophenacyl bromide | HCID 7454 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | Methanethioamide | HCID 3005587 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 4-(4-Bromophenyl)thiazole | HCID 4404138 | 95% |
Reaction Steps
To a stirred solution of phosphorus pentasulfide (24.5 g, 55 mmol) in dioxane (250 ml) was added formamide (28.4 g, 630 mmol), and the mixture was heated at reflux temperature for 2 hours. The reaction mixture was cooled down to room temperature, and the solution was decanted away from solids. To a stirred solution of 2,4′-dibromoacetophenone (15 g, 54 mmol) in dioxane (100 ml) was added the thioformamide solution, and the mixture was heated at reflux temperature for 6 hours. The reaction mixture was cooled down to room temperature, and made basic by addition of 2N NaOH aqueous solution. The whole was extracted with diethyl ether. The organic layer was washed with brine, dried over MgSO4, and concentrated in vacuo. The residue was purified by flash chromatography eluting with CH2Cl2 to give title compound (12.3 g, 95% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06608095B2 |
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| Source dataset | uspto-grants-2003_08 |
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| ORD ID | ord-d74b04dade6440be9feab2d6f247d766 |
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| Source note | uspto-grants-2003_08 |
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