Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pentane | HCID 8003 | — |
| Reactant | Carbon tetrabromide | HCID 11205 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 67128148 | HCID 67128148 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67128227 | HCID 67128227 | — |
Reaction Steps
4.44 g (16.94 mmol) triphenylphosphine in 10 ml dichloromethane is added in drops to an ice-cold solution of 3 g (12.49 mmol) [2-fluoro-5-(tetrahydropyrane-2-yloxymethyl)-phenyl]methanol and (15.61 mmol) tetrabromomethane in 30 ml anhydrous dichloromethane and stirred for another 45 minutes at 0° C. The reaction solution is mixed with pentane, the precipitation is suctioned off and washed with dichloromethane. The filtrate is washed with 5% sodium hydrogen carbonate solution, water and sodium chloride solution and dried over magnesium sulfate. After removing the solvent, the residue is purified by way of column chromatography on silica gel using diethyl ether/petrol ether 1:10.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08273793B2 |
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| Source dataset | uspto-grants-2012_09 |
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| ORD ID | ord-c9605f343bba4505bea76a7462c33638 |
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| Source note | uspto-grants-2012_09 |
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