Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Diisobutylaluminumhydride | HCID 21225700 | — |
| Reactant | HCID 86585321 | HCID 86585321 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 69556315 | HCID 69556315 | 90% |
Reaction Steps
To a solution of ethyl (E)-3-(3-nitrophenyl)-2-pentenoate (Preparation 13, 105 g, 0.43 mol) in toluene (1400 ml) at −10° C. under nitrogen was added dropwise over 3 h diisobutylaluminium hydride (1.0 M in toluene, 1 l, 1.0 mol), then the mixture was stirred at 0° C. for 1 hour. Water (400 ml) was carefully added, followed by sodium hydrogen carbonate (700 g). The resulting slurry was vigorously stirred for 10 minutes, then ethyl acetate (2 l) was added, and the mixture stirred for 1 h. The mixture was dried (MgSO4), filtered and concentrated in vacuo to give the title compound as a pale brown oil (80 g, 90%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06313312B1 |
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| Source dataset | uspto-grants-2001_11 |
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| ORD ID | ord-f6c1afcb6baf4522b1b9c085f0a00ff2 |
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| Source note | uspto-grants-2001_11 |
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