Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Iodine chloride | HCID 24640 | — |
| Reactant | Benzimidazol-2-one | HCID 162542 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 22287489 | HCID 22287489 | — |
Reaction Steps
A mixture of iodine monochloride and 2H-benzimidazole-2-one (0.67 g) (Method 59) in glacial acetic acid (8 ml) was heated to 80° C. for 1 hour then cooled. The mixture was partitioned between saturated aqueous sodium sulphite solution and DCM. The organic layer was evaporated to dryness then redissolved in ethyl acetate. The aqueous layer was extracted with ethyl acetate then all ethyl acetate extracts were combined and washed with saturated aqueous sodium hydrogencarbonate solution, water and brine. The organic extracts were passed through a Varian Chem Elut column and washed through with ethyl acetate. Volatile material was removed by evaporation to give the title compound (0.36 g) as a solid which was used without further purification. MS (ESP−): 261 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06498275B1 |
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| Source dataset | uspto-grants-2002_12 |
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| ORD ID | ord-50700de48396435e970fee060dc14725 |
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| Source note | uspto-grants-2002_12 |
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