Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | HCID 54104975 | HCID 54104975 | — |
| Product | HCID 54482468 | HCID 54482468 | — |
Reaction Steps
A solution of 1.5 g. of 3,7,7-trimethyl-2,4-octadien-1-ol in 15 ml. of acetyl ether is added dropwise at -20° C. to 1.20 g. of phosphorus tribromide. The temperature is allowed to rise to 0° C. in the course of 30 minutes and then the mixture poured onto 30 ml. of ice-water. The mixture is extracted three times with diethyl ether, the extracts washed with water, 10% by weight aqueous potassium bicarbonate solution and semi-saturated and saturated aqueous sodium chloride solution and then dried over sodium sulfate. After removal of the solvent under reduced pressure in the cold, there is obtained 1-bromo-3,7,7-trimethyl-2,4-octadiene which exhibits a spot in the thin-layer chromatogram [Rf = 0.63; hexane/ethyl acetate (4:1 parts by volume)]. This substance is used in the process without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04002647 |
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| Source dataset | uspto-grants-1977_01 |
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| ORD ID | ord-4ecdccf6c0054e1eb4a63d3d6fad1728 |
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| Source note | uspto-grants-1977_01 |
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