Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Sodium Sulfite | HCID 24437 | — |
| Reactant | Methyl 3-fluoro-4-hydroxybenzoate | HCID 7019368 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 57467610 | HCID 57467610 | — |
Reaction Steps
3.9 g of 3-fluoro-4-hydroxy-benzoic acid methyl ester were dissolved using 25 ml of acetic acid and 25 ml of DCM. The mixture was cooled to 0° C. and 1.4 ml bromine added slowly (30 minutes) at 0° C. Stirring was continued at room temperature for 18 h. Then, 200 ml of EA and a solution of 7.6 g Na2SO3 in 50 ml of water were added and the resulting mixture was stirred for 10 minutes at room temperature. The layers were separated, and the organic layer was washed using first 50 ml of water and second 50 ml of a saturated aqueous NaCl-solution. The organic layer was dried using MgSO4 and evaporated to yield 5.0 g of the title compound that was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08618304B2 |
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| Source dataset | uspto-grants-2013_12 |
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| ORD ID | ord-dde2a06914b74a9b90ebe587b4b63032 |
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| Source note | uspto-grants-2013_12 |
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