Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formamide | HCID 713 | — |
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Methanethioamide | HCID 3005587 | — |
| Reactant | HCID 22379891 | HCID 22379891 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 22379917 | HCID 22379917 | — |
Reaction Steps
A mixture of 3-(5-bromo-1-ethyl-1H-benzoimidazol-2-yl)-1-(3-fluoro-phenyl)-propan-1-one (0.2 g, 0.53 mmol) and bromine (0.1 g, 0.62 mmol) is refluxed in 1,4-dioxane for 2 hours. Thioformamide (freshly made from formamide and P2S5 in 1,4-dioxane) (1.3 mmol) are added to the solution. The mixture is refluxed overnight. The solvent is removed and NaHCO3 (aq.) (15 mL) and DCM (40 mL) are added to the residue. The organic layer is separated and the aqueous layer is extracted with DCM (2×30 mL). The combined organic layers are dried and solvent removed. The crude is purified by PTLC (5% methanol in DCM) to give 5-bromo-1-ethyl-2-[4-(3-fluoro-phenyl)-thiazol-5-ylmethyl]-1H-benzoimidazole. 1H NMR (CDCl3) δ 8.78 (s, 1H), 7.91 (s, 1H), 7.38-7.48 (m, 4H), 7.11-7.19 (m, 2H), 4.59 (s, 2H), 3.90 (q, 2H), 1.12 (t, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06916819B2 |
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| Source dataset | uspto-grants-2005_07 |
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| ORD ID | ord-7df2671c8b964a4f9734700f463209d0 |
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| Source note | uspto-grants-2005_07 |
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