Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzyl Bromide | HCID 7498 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Reactant | Diisopropyl (R)-(+)-malate | HCID 10921962 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 10957810 | HCID 10957810 | 69.1% |
Reaction Steps
To a cold (−78° C.) solution of diisopropyl-(R)-(+)-malate (9.4 mL; 45.82 mmol; 1.00 eq.) in anhydrous THF (17 mL) was added slowly a solution (1 M) of lithium bis(trimethylsilyl)amide (96.2 mL; 1.00 M; 96.2 mmol; 2.10 eq.) in THF. The temperature was raised to 20° C. over 30 minutes, than lowered again to −78° C. Benzyl bromide (9.40 g; 55.0 mmol; 1.20 eq.) was added and the mixture stirred at RT for 16 hours. The reaction mixture was then cooled to 0° C. and a saturated solution of NH4Cl was added. The resulting mixture was diluted with water, extracted three times with EtOAc. The combined organic layers were washed with brine and dried over MgSO4, filtered and evaporated under reduced pressure. The residue was then purified by chromatography (SiO2, 20/80 EtOAc/c-hex) to give the product as a colourless oil (9.76 g, 69%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08008302B2 |
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| Source dataset | uspto-grants-2011_08 |
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| ORD ID | ord-30ce48355336497ea5306276f9d5c590 |
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| Source note | uspto-grants-2011_08 |
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