HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzyl Bromide → HCID 53971539, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzyl Bromide | HCID 7498 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 54249029 | HCID 54249029 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 53971539 | HCID 53971539 | 94.6% |
Reaction Steps
To a mixture of (2-hydroxy-5-iodo-phenyl)-phosphonic acid diethyl ester (14.7 g, 41.2 mmol) and cesium carbonate, (17.4 g, 53.5 mmol) in DMF (150 mL) was added benzyl bromide (6.40 mL, 54 mmol). The reaction was allowed to stir for 2.5 days at rt at which point the reaction was concentrated under reduced pressure, the residue diluted in 0.5 N HCl (30 mL) and extracted twice with EtOAc. The pooled organic extracts were washed with brine, dried over anhydrous Na2SO4 and concentrated under reduced pressure to give 17.4 g (91%) of a colorless solid after recrystallization (EtOAc-hexanes). Rf 0.36 (1:1 EtOAc-hexanes). Electrospray Mass Spectrum (50/50 acetonitrile/water) m/z 447 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06482852B2 |
| Source dataset | uspto-grants-2002_11 |
| ORD ID | ord-f7d54a6bcdcb4e57bc7fcfe50394a045 |
| Source note | uspto-grants-2002_11 |