HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-bromobutanimide → Methyl 4-bromo-5-methoxythiophene-2-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | Methyl 5-Methoxy-2-thiophenecarboxylate | HCID 12646617 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Methyl 4-bromo-5-methoxythiophene-2-carboxylate | HCID 57826524 | 75.4% |
Reaction Steps
NBS (903 mg, 5.07 mmol) was added in portions to a 5 mL sealed tube reactor containing methyl 5-(methyloxy)-2-thiophenecarboxylate (0.73 g, 4.23 mmol) in N,N-Dimethylformamide (DMF) (20 mL) at room temperature and the reaction stirred for 1 hour. Additional NBS (249 mg) was added and after 1 h at room temperature the product was partitioned between CHCl3 and H2O. The organic layer was dried with Na2SO4, adsorbed onto silica and purified via column chromatography (0-25% EtOAc/Hexanes) affording the title compound (825 mg, 3.19 mmol, 75%): LC-MS (ES) m/z=252 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08410158B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-c775799a7a1b41bc94d0ef8ba1580f0f |
| Source note | uspto-grants-2013_04 |