HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon tetrabromide → HCID 22407359, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon tetrabromide | HCID 11205 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 54431298 | HCID 54431298 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22407359 | HCID 22407359 | — |
Reaction Steps
28.6 g (0.1 mol) of 4-(α-ethoxycarbonyl-benzyloxy)benzyl alcohol are dissolved in 300 ml of dichloromethane and mixed with 31.6 g (0.12 mol) of triphenylphosphine. Whilst cooling with ice, a solution of 40.0 g (0.12 mol) of carbon tetrabromide in 100 ml of dichloromethane is added dropwise. The mixture is stirred for 30 minutes at ambient temperature and then concentrated by evaporation. The residue is purified over a silica gel column (particle size: 0.063-0.02 mm), using as eluant first petroleum ether and then mixtures of petroleum ether and ethyl acetate of increasing polarity (9:1 and 8:2). The unified fractions are evaporated down in vacuo.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05519138 |
| Source dataset | uspto-grants-1996_05 |
| ORD ID | ord-8d3c2d046611493898849adc4a0f529a |
| Source note | uspto-grants-1996_05 |