HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → Methyl 4-bromo-1H-pyrrole-2-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | 1-(4-bromo-1H-pyrrol-2-yl)-2,2,2-trichloroethanone | HCID 2798140 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Solvent | Water | HCID 962 | — |
| Product | Methyl 4-bromo-1H-pyrrole-2-carboxylate | HCID 2763594 | 85% |
Reaction Steps
To a solution of Example 1B (20 g, 68 mmol) in methanol (100 mL), a solution of NaOMe (1M in MeOH, 34 mL, 34 mmol) was added slowly. This mixture was then stirred at ambient temperature for 1 h after which it was diluted with water (300 mL) and the organic layer was separated. The aqueous phase was extracted with CH2Cl2 and the combined organic layer and extracts were washed with water (2×50 mL), dried (MgSO4) and evaporated under reduced pressure. Recrystallization of the residue from hexane gave 4-Bromo-2-methoxycarbonylpyrrole (Example 1C, 12 g, 85%) as a white solid. LC-MS, [M−H]+=203. 1H NMR (DMSO-d6, 400 MHz): δ 12.31 (brs, 1H), 7.16 (s, 1H), 6.81 (s, 1H), 3.75 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08580959B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-aca1a93d9b8d486397a3ddff3a3138e9 |
| Source note | uspto-grants-2013_11 |