Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Reactant | HCID 22054484 | HCID 22054484 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 54711424 | HCID 54711424 | 28% |
Reaction Steps
N,N′-Bis-(3-iodo-4-methyl-phenyl)-malonamide (43.4 g, 81.3 mmol) was added portionwise to a melt of aluminum chloride (32.5 g, 244 mmol) and sodium chloride (9.50 g, 163 mmol) at 150° C., then the mixture was heated at 250° C. for 20 min. After cooling the solid formed was suspended in hot water and collected by filtration. This crude material was suspended in hot 0.5 M aq. sodium hydroxide solution, insoluble material was removed by filtration, and the filtrate was acidified with 25% aq. hydrochloric acid solution. The precipitate was collected by filtration, washed with water and ethyl acetate, and dried to afford the title compound (6.85 g, 28%). Light brown solid, EI-MS: m/e=301.2 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07012073B2 |
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| Source dataset | uspto-grants-2006_03 |
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| ORD ID | ord-519baf2b4fa1480c884ad448671be7e8 |
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| Source note | uspto-grants-2006_03 |
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