Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | 4-Chlororesorcinol | HCID 1731 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86645267 | HCID 86645267 | 46% |
Reaction Steps
To a flame-dried 50 mL round-bottom flask is weighed 4-chlororesorcinol (1.44 g, 10 mmole) and diethyl-1,3-acetonedicarboxylate (1.82 mL, 10 mmole) and trifluoroacetic acid (10.0 mL) added. This mixture is heated to reflux (98° C.) in an oil-bath for 18 hours, cooled to room-temperature and poured into ice-water (100 mL) with stirring for 1 hour. The resulting off-white precipitate is filtered and washed with ice-cold water, dried in air and in vacuo overnight to give a yellow crystalline powder (1.29 g, 4.56 mmole, 46%) TLC (irrigant=7:3 ethylacetate:methanol, Rf=0.86).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08460862B2 |
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| Source dataset | uspto-grants-2013_06 |
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| ORD ID | ord-5efa938ccc2f4140abcea8571900b790 |
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| Source note | uspto-grants-2013_06 |
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