HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Sulfite → tert-Butyl (2S)-2-(5-bromo-1H-imidazol-2-yl)pyrrolidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Sulfite | HCID 24437 | — |
| Reactant | (S)-tert-Butyl 2-(4,5-dibromo-1H-imidazol-2-yl)pyrrolidine-1-carboxylate | HCID 56605191 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | tert-Butyl (2S)-2-(5-bromo-1H-imidazol-2-yl)pyrrolidine-1-carboxylate | HCID 56605192 | 52.2% |
Reaction Steps
A mixture of Example 126D (12.5 g, 31.5 mmol) in dioxane (400 mL) and H2O (400 mL) had a solution of Na2SO3 (43.7 g, 347 mmol) in H2O (400 mL) added and was heated to reflux for 21 hours. The mixture was concentrated to half volume and extracted with CH2Cl2 (3×200 mL). The organic was then washed with brine, dried (MgSO4), filtered and concentrated. Purification by trituration (CH2Cl2, tBuOMe, and Hexanes) afforded 5.2 g (52%) of the title compound. MS (ESI) m/z 317 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09006387B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-7c969584d9524f179dc112d77edaa2b3 |
| Source note | uspto-grants-2015_04 |