HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → (4-Bromothiophen-2-yl)(cyclopropyl)methanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Cyclopropyl-2-thienylmethanone | HCID 80328 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | (4-Bromothiophen-2-yl)(cyclopropyl)methanone | HCID 59332599 | — |
Reaction Steps
Cyclopropyl(2-thienyl)methanone (Aldrich, 1.5 g, 9.9 mmol) was diluted in chloroform (10 mL). Aluminum chloride (2.96 g, 22.2 mmol, 2.3 eq) was added, followed by the dropwise addition of bromine (0.56 mL, 11 mmol, 1.1 eq) in chloroform (10 mL). The mixture was stirred at rt overnight, then poured onto ice water (100 mL). The whole was extracted with dichloromethane, and the combined organic layers were dried over sodium sulfate, filtered, and concentrated to give brown oil. The crude product was purified by isco combiflash, 120 g column, eluting with 0-15% ethyl acetate in hexanes. Yellow oil was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071584B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-83c896806e754338bf7fbc1857a04d6a |
| Source note | uspto-grants-2011_12 |