Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 22168209 | HCID 22168209 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 14722383 | HCID 14722383 | 82.1% |
Reaction Steps
In 20 ml of pyridine was dissolved 4.81 g of 3,3-dibromo-2,3-dihydro-7-methylsulfonylamino-6phenoxy-4H-1-benzopyran-4-one. The solution was refluxed for 20 minutes. The reaction mixture was introduced into 200 ml of water. The mixture was adjusted to pH 4 with concentrated hydrochloric acid and then extracted with two 100-ml portions of ethyl acetate. The extracts (the organic layers) were combined, washed with water and a saturated aqueous sodium chloride solution in this order, and dried with anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The resulting crystal was recrystallized from acetonitrile to obtain 3.30 g (yield: 82%) of 3-bromo-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran-4-one having a melting point of 215°-216° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04954518 |
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| Source dataset | uspto-grants-1990_09 |
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| ORD ID | ord-9eafcfcd70854aac83658c18336f1968 |
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| Source note | uspto-grants-1990_09 |
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