Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | HCID 16756661 | HCID 16756661 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 16756984 | HCID 16756984 | 75.3% |
Reaction Steps
To a solution of [3-(4-chlorophenyl)-[1,2,4]thiadiazol-5-yl]-methanol (0.25 g, 1.10 mmol) in toluene (8 ml) was added PBr3 (0.17 ml, 1.65 mmol). The resulting reaction mixture was refluxed at 120° C. for 15 min. After the completion of the reaction (TLC monitoring), the reaction mixture was cooled to 0° C., added water (50 ml) and extracted with ethyl acetate (3×50 ml). The combined organics was washed with saturated NaHCO3 solution, dried over Na2SO4, filtered and concentrated under vacuum. The crude residue was purified over silica gel (100-200 M, 2% EtOAc-Hexane) to get the desired product (0.24 g, 75%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08415383B2 |
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| Source dataset | uspto-grants-2013_04 |
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| ORD ID | ord-654b535c1deb4af1940fa6902bbcfe54 |
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| Source note | uspto-grants-2013_04 |
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