Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Boron trifluoride | HCID 6356 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 18982045 | HCID 18982045 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18982044 | HCID 18982044 | 30% |
Reaction Steps
4.4 ml of fleshly distilled boron trifluoride are added dropwise, while cold, to 1.1 g of dry sodium borohydride suspended in 35 ml of freshly distilled tetrahydrofuran. The reaction mixture is stirred at 0° C. for 2 hours and then 3.5 g (0.01 mol) of the compound obtained in Step g in 100 ml of tetrahydrofuran are added. The mixture is then heated under reflux for one hour and then 50 ml of a 2N hydrochloric acid solution are added while cold. The mixture is neutralised with sodium hydroxide and then extracted with ether. Customary treatment of the organic phase yields a crude product which is purified over a silica gel column (eluant: trichloromethane). 1 g of the pure desired product is obtained in the form of a colourless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05500426 |
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| Source dataset | uspto-grants-1996_03 |
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| ORD ID | ord-529b7b2b7ef24a2bbc3fb28329d16819 |
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| Source note | uspto-grants-1996_03 |
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