Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 67272898 | HCID 67272898 | — |
| Product | HCID 67273043 | HCID 67273043 | 60% |
Reaction Steps
A mixture of 190 mg (0.753 mmol) of 7-(2-ethylphenyl)-1-methyl-1,3-dihydro-2H-benzimidazol-2-one and 1.5 mL of phosphorus oxychloride was stirred at 80° C. for 5 hours. After cooling, the reaction mixture was poured into ice and neutralized by 12 N sodium hydroxide. The aqueous suspension was extracted with ethyl acetate (X2). The combined organic layer was washed with brine (X1), dried over sodium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with a 3-10% ethylacetate/n-hexane gradient mixture to give 123 mg (60%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08163935B2 |
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| Source dataset | uspto-grants-2012_04 |
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| ORD ID | ord-fae8eb71bb244c148d725b37a9193017 |
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| Source note | uspto-grants-2012_04 |
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