Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Diisobutylaluminum hydride | HCID 14487 | — |
| Reactant | HCID 11392096 | HCID 11392096 | — |
| Product | HCID 11369822 | HCID 11369822 | — |
Reaction Steps
A solution of 2-(5-bromo-2-chloro-4-methoxy-phenyl)-2-methyl-propionitrile (13 g, 0.045 mol) in dry THF (80 mL) was cooled to −10° C. under argon. DIBALH (1M in THF, 100 mL, 0.10 mol) was added keeping the temperature below 0° C. The mixture was stirred for 30 min/0° C. and then 2 h/25° C. The clear solution was carefully poured into icecold hydrochloric acid (2M, 100 mL). The THF was removed under reduced pressure. The aqueous phase was cooled and the crude product was filtered off and recrystallized from boiling MeOH. Yield: 7.8 g (59%). GCMS: >99%
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07642367B2 |
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| Source dataset | uspto-grants-2010_01 |
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| ORD ID | ord-3cc16568cda94b7388620af0faccd3a2 |
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| Source note | uspto-grants-2010_01 |
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