Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | 4-Bromo-5-nitrophthalide | HCID 18551185 | — |
| Catalyst | Ferrous Sulfate | HCID 24393 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 4-Bromo-5-aminophthalide | HCID 18551168 | 70.3% |
Reaction Steps
6.6 g of 4-bromo-5-nitrophthalide is dissolved in 45 ml of ethanol and added in drops to a mixture of 65 g of iron(II) sulfate, 220 ml of water and 65 ml of ammonia (33%) that is heated to 60° C. and stirred well. After 2 hours at 60° C., the mixture is absorptively precipitated five times with 200 ml of diethyl ether. The diethyl ether phases are concentrated by evaporation. As a residue, 4.1 g of 4-bromo-5-aminophthalide is obtained, melting point 176-180° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06245804B1 |
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| Source dataset | uspto-grants-2001_06 |
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| ORD ID | ord-417ce4b9c1f746f295dbae1f9e4e0612 |
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| Source note | uspto-grants-2001_06 |
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