Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | HCID 118598814 | HCID 118598814 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 118598739 | HCID 118598739 | — |
Reaction Steps
To a stirred solution of hydrogenbromide (1.43 g, 15.24 mmol) in acetic acid in 1,4-dioxane (30 mL), 6-bromo-8-chloro-1′,4′-ditosyl-2H-spiro[imidazo[1,5-a]pyridine-3,6′-[1,4]diazepane]-1,5-dione (1 g, 1.52 mmol) was added at room temperature. The vial was sealed and heated the reaction mass to 100° C. for 16 h. After completion, solvent was removed under reduced pressure and crude was triturated with dichloromethane to afford 6-bromo-8-chloro-2H-spiro[imidazo[1,5-a]pyridine-3,6′-[1,4]diazepane]-1,5-dione (4) as brown solid. Yield: 0.5 g, 94%; MS (ESI) m/z 362.28 [M+1]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09382248B2 |
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| Source dataset | uspto-grants-2016_07 |
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| ORD ID | ord-4a59d44f27f34bfeacf167c7ebe7951a |
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| Source note | uspto-grants-2016_07 |
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