Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 9859781 | HCID 9859781 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 9859510 | HCID 9859510 | — |
Reaction Steps
Under argon, the compound obtained in Example 1 (342 mg; 1.37 mmol) is dissolved in 8 ml of distilled dichloromethane. The solution is cooled to −78° C., and then boron tribromide (4 eq.; 5.47 mmol; 5.17 μl) diluted with 5 ml of dichloromethane is slowly added. The mixture is left for one hour at −78° C. and then for 2 hours at ambient temperature. The reaction mixture is hydrolysed to pH 7 with a saturated sodium hydrogen carbonate solution and then the aqueous phase is extracted 4 times with dichloromethane. The organic phases are combined, and then removed under reduced pressure. The solid obtained is dissolved in a minimum amount of dichloromethane, precipitated in the presence of pentane, filtered, and then washed with an Et2O/pentane mixture.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06620809B2 |
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| Source dataset | uspto-grants-2003_09 |
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| ORD ID | ord-4e4487b04ed4426b9dfd75a1f39fcce2 |
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| Source note | uspto-grants-2003_09 |
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