HuagongsheHuagongshe Chemistry Print Report · For research reference only
5-Bromo-1-indanone → (E)-5-bromo-1-(methoxymethylene)-2,3-dihydro-1H-indene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 5-Bromo-1-indanone | HCID 520695 | — |
| Reactant | Methoxymethyl-triphenylphosphonium chloride | HCID 2723798 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (E)-5-bromo-1-(methoxymethylene)-2,3-dihydro-1H-indene | HCID 58909702 | 93.2% |
Reaction Conditions
| Temperature | -20 °C |
|---|
Reaction Steps
To a suspension of (methoxymethyl)triphenylphosphonium chloride (39.7 g, 116 mmol) in THF (210 ml) at −20° C. was added dropwise 1M potassium t-butoxide (95 ml, 95 mmol) and the solution stirred at −20° C. for 20 min. To this solution was added dropwise a solution of 5-bromo-2,3-dihydro-1H-inden-1-one (10.0 g, 47.4 mmol) in THF (230 ml) and stirring was continued at −20° C. for 30 min then warmed to room temperature and stirred for 2 h. The solution was filtered through Celite and the filtrate was concentrated in vacuo to give crude product which was purified by chromatography on a silica gel cartridge eluting with CH2Cl2/hexane to give the title compound (10.56 g, 93%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08415351B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-7af8363d16b04b9dbe2d74c608f8d779 |
| Source note | uspto-grants-2013_04 |