Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Bis(trifluoroacetoxy)iodobenzene | HCID 102317 | — |
| Reactant | 2-Ethyl-1,3-benzoxazol-4-amine | HCID 12071589 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Diisopropyl Ether | HCID 7914 | — |
| Solvent | Acetonitrile--water (1/1) | HCID 18373917 | — |
| Product | 2-Ethyl-4,7-benzoxazoledione | HCID 12071590 | — |
Reaction Steps
A solution of [bis(trifluoroacetoxy)iodo]benzene (2.2 eq.) in a mixture of acetonitrile and water (80/20) is added dropwise to a solution of 2-ethyl-1,3-benzoxazol-4-amine (1 eq.) in the same acetonitrile/water mixture maintained at −5° C. The reaction medium is then diluted with water followed by extracting with dichloromethane. The resulting organic phase is washed with water, followed by drying over sodium sulphate and concentrating in order to produce a brown paste. Purification by medium pressure chromatography on silica gel produces, after taking up in diisopropyl ether, a yellow crystalline solid. Melting point: 99° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07495021B2 |
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| Source dataset | uspto-grants-2009_02 |
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| ORD ID | ord-ecd578abf75749c6a5e3b351c760ec2e |
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| Source note | uspto-grants-2009_02 |
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