HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 59278516, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | Methyl pyrrole-2-carboxylate | HCID 136930 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Product | HCID 59278516 | HCID 59278516 | — |
Reaction Steps
To a solution of methyl 1H-pyrrolecarboxylate (4.00 g, 32.00 mmol) in dioxane was added anhydrous sodium acetate (4.92 g, 60.00 mmol) followed by a solution of bromine (32.00 mmol) in dioxane (150 mL) dropwise. After 4 hours, the solvent was concentrated in vacuo and the residue was poured into an ice cold solution of 5% aqueous sodium carbonate (100 mL) and extracted with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate and concentrated in vacuo. The residue was purified by silica gel chromatography eluting with 10-40% ethyl acetate in heptane. The major fractions were combined and the solvent was concentrated in vacuo to afford the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08063065B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-c07bec77832f4a72af50c19918d8d2d5 |
| Source note | uspto-grants-2011_11 |