Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Carbon tetrabromide | HCID 11205 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Benzenebutanal, 3-methoxy- | HCID 10821200 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 21221331 | HCID 21221331 | 94.8% |
Reaction Steps
To a solution of carbon tetrabromide (16.7 g)in methylene chloride (35 ml) was added triphenyiphosphine (26.0 g) in methylene chloride (35 ml) at 0° C. and the mixture was stirred for 10 min. To the mixture was added a solution of 1-(3-formylpropyl)-3-methoxybenzene (3.00 g) in methylene chloride (20 ml) at 0° C. The mixture was stirred for 30 min at 0° C. To the mixture was added gradually n-hexane and the mixture was filtered to remove triphenylphosphineoxide. The filtrate was washed with water and a saturated aqueous solution of sodium chloride, successively, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=24:1) to give the title compound (5.33 g) having the following physical data.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05378716 |
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| Source dataset | uspto-grants-1995_01 |
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| ORD ID | ord-a07a1e1117fb416dbc241761cadc5863 |
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| Source note | uspto-grants-1995_01 |
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