HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,3-Dibromo-5,5-dimethylhydantoin → HCID 59231934, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,3-Dibromo-5,5-dimethylhydantoin | HCID 6479 | — |
| Reactant | HCID 59232074 | HCID 59232074 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59231934 | HCID 59231934 | 188.1% |
Reaction Steps
A solution of tert-butyl 3-(4-aminopyrrolo[2,1-f][1,2,4]triazin-7-yl)pyrrolidine-1-carboxylate (1.2 g, 3.96 mmol) in DMF (20 mL) was cooled to 40° C. and treated with 1,3-dibromo-5,5-dimethylhydantoin (508 mg, 1.78 mmol). The reaction was allowed to warm slowly to rt over a 2 h period and was then partitioned between EtOAc and bicarbonate solution. After concentration, the residue was triturated with EtOAc to yield the desired product (1.28 g, 85%). 1H-NMR (DMSO): δ 7.86 (s, 1H), 6.69 (s, 1H), 3.68 to 3.80 (m, 2H), 3.36 to 3.46 (m, 1H), 3.20 to 3.30 (m, 2H), 2.16 to 2.30 (m, 1H), 1.98 to 2.08 (m, 1H), 1.37 (s, 9H); MS: LC/MS (+esi), m/z=382.1 [M+H]; LC/MS rt=3.08 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08143393B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-d6895d71fc654f03b135b414441a3e45 |
| Source note | uspto-grants-2012_03 |