Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | 2-Phenyl-4-(4-hydroxymethylphenoxy)ethyloxazole | HCID 15487822 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15487823 | HCID 15487823 | 92% |
Reaction Steps
To a suspension of 2-phenyl-4-(4-hydroxymethylphenoxy)ethyloxazole (30 g, 102 mmol) in 300 mL of methylene chloride at 5° C. under a nitrogen atmosphere was added phosphorous tribromide (10.02 mL, 107 mmol) dropwise keeping the temperature of the reaction below 20° C. The resulting solution was allowed to stir for about 2 hours at room temperature. The reaction was cooled to about 10° C. and 20 mL of methanol was added. After about 5 minutes, the solvent was removed and the solid remaining was partitioned between 1.35 L of ethyl acetate and 1.05 L of cold 5% aqueous sodium bicarbonate. The organics were washed with another 1.05 L of 5% aqueous sodium bicarbonate, dried over magnesium sulfate, filtered, and removed to give 33.3 g of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06353027B1 |
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| Source dataset | uspto-grants-2002_03 |
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| ORD ID | ord-a1500cc1ec814570baa01bef1407c2dd |
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| Source note | uspto-grants-2002_03 |
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