Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | O-Xylene | HCID 7237 | — |
| Reactant | 2,4,6-Trimethylpyridine | HCID 7953 | — |
| Reactant | HCID 13826525 | HCID 13826525 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 13826528 | HCID 13826528 | — |
Reaction Steps
A mixture of 0.605 g. (0.0010 mole) of [1α,3β,7ξ,24R]-7-bromo-24-fluorocholest-5-en-1,3,25-triol 1,3-diacetate, 0.6 ml. of s-collidine and 18 ml. of xylene was heated at reflux (140° C.) for 0.5 hr and cooled. The mixture was diluted with 30 ml. of toluene. This solution was washed with 10% aqueous sulfuric acid, and saturated aqueous sodium bicarbonate solution. The organic phase was dried over anhydrous magnesium sulfate, filtered, and evaporated to dryness. The residue was purified by column chromatography on 0.06-0.20 mm silica gel to yield [1α,3β,24R]-24-fluorocholesta-5,7-dien-1,3,25-triol 1,3-diacetate, [α]D23 -21° (c 0.5, CHCl3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04652405 |
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| Source dataset | uspto-grants-1987_03 |
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| ORD ID | ord-a5f1d6717dde4aed878071c92a9876fb |
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| Source note | uspto-grants-1987_03 |
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